CN109759029A - A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent and preparation method thereof - Google Patents
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of magnetic graphene polystyrene complex microsphere sewage-treating agents, which is characterized in that passes through modified nanometer Fe3O4Processing is modified to polystyrene microsphere with graphene oxide, a kind of magnetic graphene polystyrene complex microsphere is made, adsorption mechanism: can quickly capture the heavy metal ion in simultaneously strong adsorption sewage, especially Pb micro in sewage2+、Cr6+、Cu2+、Hg2+Deng, selective strong, adsorption efficiency height, and graphene oxide and polystyrene microsphere can generate strong complexing to metal ion, therefore the heavy metal ion adsorbed is not easily to fall off.
Description
Technical field
The present invention relates to a kind of magnetic polystyrene microsphere sewage-treating agents, and in particular to poly- to a kind of magnetic graphene
Styrene complex microsphere sewage-treating agent and preparation method thereof, belongs to technical field of sewage.
Technical background
According to statistics in the annual sewage discharge in the whole nation, only 10% sanitary sewage and 70% trade effluent are handled, and
Wherein there are about the water outlets of half Industrial Waste Water Treatments facility, and national emission standard is not achieved, remaining untreated sewage is then direct
It is discharged into rivers and lakes, the water environment in China is caused to be subject to serious pollution and destroy；The discharge amount of town domestic sewage just with
City-building and development and in incremental trend.Wherein the high volence metal ion in rivers and lakes (including toxic metals from
Son) content is higher and higher, in the sewage of the discharges such as part Ceramics Enterprises, iron and steel enterprise, chemical company, Pb2+、Cr6+Deng serious
Exceeded, effluent problem especially heavy metal ions in sewage excessive problem is urgently to be resolved.
In order to solve the problems, such as the processing of waste water, existing method has a variety of methods such as physics, chemistry, biology, synthesis,
About the novel invention in terms of sewage treatment open.
China Patent No. CN201610017517.0 discloses a kind of compound sewage-treating agent and preparation method thereof, with two
Five methylenephosphonic acid of ethylene triamine, sodium lignin sulfonate, polyacrylamide, sodium nipagin esters and polymeric aluminium ferrum silicate are chelating agent
Or coagulation agent, realize pollutant sedimentation；This method preparation method is simple and reliable, and product obtained can effectively handle oilfield sewage,
With good catharsis, and product is environmentally friendly, and water treatment agent usage amount is small, excellent effect, application easy to spread.
China Patent No. CN201410134380.8 disclose it is a kind of using autocatalyzed oxidation as the PCB copper-containing wastewater of core at
The pH of alkalinity complexing copper waste water is adjusted to weakly acidic pH or neutrality using acidic copper-containing waste water, utilizes Zero-valent Iron by reason method, this method
By the newborn elemental copper of for the benefit of subsequent Fenton reaction of the copper ion partial reduction in waste water, in ferrous iron, newborn elemental copper
Concerted catalysis effect under, realize efficient Fenton reaction in neutral conditions to contact break, be followed by Zero-valent Iron reduction realize it is useless
The recycling of copper ion in water, water outlet removes ferrous iron and ferric ion by the method that alkali tune precipitates, while utilizing iron hydrogen-oxygen
Flocculation, the suction-operated of compound further go water removal in pollutant, final outflow water copper ion concentration be lower than 0.5mg/L, iron from
Sub- concentration is lower than 10mg/L, and biodegradability is good.The present invention makes full use of copper present in system, utilizes while copper removal
The catalytic action of copper significantly reduces the dosage of acid, alkali, reduces water outlet salt content, has industrial application value.
On the whole, about in the existing disclosed patent of sewage treatment, sewage-treating agent to the absorption of heavy metal ion,
There are the disadvantages such as poor selectivity, sensitivity be low for complexing, and trace level content is enough to generate human body the Pb of injury2+、Cr6+Nothing
The processing of method specific aim.
Magnetic macromolecular microsphere be inorganic particle is formed in conjunction with high-molecular organic material one kind it is compound micro-
Ball is novel functional material；Polymer composite microsphere has variable grain form and surface characteristics, because it is with specific surface
Greatly, strong adsorption, agglutination is big and has the characteristics such as surface respond, biotechnology, biology doctor can be widely used in
In terms of medicine engineering, sewage treatment, at cell separation, Protein Separation, targeted drug, biochemical analysis and heavy metal containing sewage
Reason.
Magnetic microsphere is used as flocculant at present and adsorbent carries out wastewater treatment primarily directed to chitosan magnetic microsphere.
Chitosan is unique alkaline polysaccharide existing for nature, its amido easily forms quaternary ammonium compound cation, there is weakly-basic anion
Exchange interaction, due to the presence of free amine group, chitosan class has the dielectric property of cationic poly in an acidic solution,
It can be used as flocculating agent, but can dissolve in an acidic solution, stability is poor.Therefore, graphene oxide and magnetic polystyrene are done
The heavy metal ion sewage that trace level is handled at complex microsphere is research direction from now on.
Summary of the invention
To overcome the problems, such as that existing sewage-treating agent counterweight metalloform-selective is poor, the present invention proposes a kind of magnetic stone
The preparation method of black alkene polystyrene complex microsphere sewage-treating agent.
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent of the invention, which is characterized in that pass through modification
Nanometer Fe3O4Being modified processing to polystyrene microsphere with graphene oxide, that a kind of magnetic graphene polystyrene is made is multiple
Microballoon is closed, adsorption mechanism: utilizing the heavy metal ion and graphene oxide and polyphenyl in magnetic iron oxide capture sewage
Ethylene microballoon inhales the strong absorption complexing power of metal ion strongly under the synergistic effect of three to heavy metal ion
It is attached and not easily to fall off.
A kind of preparation method of magnetic graphene polystyrene complex microsphere sewage-treating agent, its step are as follows:
A), chemical precipitation method prepares nanometer Fe3O4Particle: under nitrogen protection, the FeCl for being 0.1mol/L by concentration3With
Concentration is the FeCl of 0.1mol/L21:1 is added in reactor solution in molar ratio, instills concentration while stirring at 30 DEG C
Stop reaction for the sodium hydroxide solution of 1mol/L, when until pH value is close to 11；Then 60 DEG C of stirring curing 1h are warming up to, are stopped
It is stood after only stirring, isolates Fe with NdFeB magnetic filter3O4, replace washing 4~6 times with distilled water and dehydrated alcohol, directly
To pH=7, dry 12h, obtains the nanometer Fe at 60 DEG C of vacuum3O4Particle；
B), nanometer Fe3O4Magnetic current is modifies: in the container equipped with 200.0~300.0 parts of ethyl alcohol, addition 20.0~
25.0 part nanometer Fe3O4Particle and 30.0~45.0 parts of polyethylene glycol, are warming up at 60 DEG C and quickly stir 3h, quiet under high-intensity magnetic field
3~5h of layering is set, supernatant liquid is removed, 200.0~250.0 parts of deionized waters are then added, disperses 15min with ultrasonic wave, then
Mechanical stirring for 24 hours, obtains modified Fe3O4Water-based magnetic fluid；
C), magnetic oxygenated graphene complex microsphere is prepared: in four mouthfuls of reactions equipped with thermometer, blender and condenser pipe
In device, under nitrogen protection, 30.0~60.0 parts of ethyl alcohol and 25.0~40.0 parts of deionized waters and 0.5~3.5 part of dispersion are added
Then agent, stirring sequentially add 0.1~0.4 part of initiator A IBN, 15.0~30.0 parts of styrene, 1.0~5.0 parts to dissolving
Carboxylic monomer, 3.0~10.0 parts of MODIFIED Fes3O4Magnetic fluid and 2.0~5.0 parts of graphene oxides after being stirred until homogeneous, surpass
Sound wave stands 2~4h after dispersing 5~10min；It starts and stirs and be warming up to 70 DEG C of holding 6~8h of isothermal reaction, then be warming up to 85
DEG C reaction 1h；Product NdFeB filter is separated, the HCl that 1mol/L is added impregnates for 24 hours to remove not wrapped Fe3O4
Particle filters, obtains institute up to 12h dry at pH=7,60 DEG C of vacuum with distilled water and dehydrated alcohol alternately washing 3~5 times
The magnetic graphene polystyrene complex microsphere sewage-treating agent stated.
The carboxylic monomer is acrylic acid, methacrylic acid, itaconic acid, maleic anhydride, N, N '-di-2-ethylhexylphosphine oxide third
At least one of acrylamide.
The dispersing agent is polyvinylpyrrolidone, alkyl phenol polyoxyethylene ether, polyethylene glycol, polyacrylic acid, polyethylene
One of alcohol is a variety of, preferably polyvinylpyrrolidone.
The graphene oxide is prepared by Hummers method, Staudenmaier method, electrochemical process or Brodie method；It is preferred that
For the graphene oxide of Hummers method preparation.
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent of the present invention can quickly capture simultaneously strong adsorption
Micro Pb in heavy metal ion in sewage, especially sewage2+、Cr6+、Cu2+、Hg2+Deng, selectivity is strong, adsorption efficiency is high,
And graphene oxide and polystyrene microsphere can generate strong complexing, therefore the heavy metal ion adsorbed to metal ion
It is not easily to fall off.
Specific embodiment
Below with reference to embodiment to the application to a kind of magnetic graphene complex microsphere sewage-treating agent of the invention make into
The detailed description of one step.It is understood that specific embodiment described herein is used only for explaining related invention, rather than
Restriction to the invention.
Embodiment 1
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent, preparation step are as follows:
A), chemical precipitation method prepares nanometer Fe3O4Particle: under nitrogen protection, by 16.2 parts of FeCl3With 12.7 parts of FeCl2
It is added in 1000L deionized water, the sodium hydroxide solution that concentration is 1mol/L is instilled while stirring at 30 DEG C, until pH value
Stop reaction when close to 11；Then 60 DEG C of stirring curing 1h are warming up to, are stood after stopping stirring, with NdFeB magnetic filter point
Separate out Fe3O4, with alternately washing 5 times of distilled water and dehydrated alcohol, until pH=7, dry 12h at 60 DEG C of vacuum is obtained described
Nanometer Fe3O4Particle；
B), nanometer Fe3O4Magnetic current is modifies: in the container equipped with 200.0 parts of ethyl alcohol, 20.0 parts of nanometer Fes are added3O4
Particle and 30.0 parts of polyethylene glycol, are warming up at 60 DEG C and quickly stir 3h, the stratification 3h under high-intensity magnetic field, remove upper liquid
Then 200.0 parts of deionized waters are added in body, disperse 15min with ultrasonic wave, then mechanical stirring is for 24 hours, obtains modified Fe3O4Water
Based magnetofluid；
C), magnetic oxygenated graphene complex microsphere is prepared: in four mouthfuls of reactions equipped with thermometer, blender and condenser pipe
In device, under nitrogen protection, be added 40.0 parts of ethyl alcohol and 25.0 parts of deionized waters and 2.0 parts of PVP, stirring to dissolving, then according to
0.25 part of initiator A IBN of secondary addition, 20.0 parts of styrene, 3.0 parts of methacrylic acids, 5.0 parts of MODIFIED Fes3O4Magnetic fluid and 3.0
Part graphene oxide after being stirred until homogeneous, stands 3h after ultrasonic wave dispersion 10min；It starts and stirs and be warming up to 70 DEG C of holdings perseverances
Temperature reaction 6h, then it is warming up to 85 DEG C of reaction 1h；By product with NdFeB filter separate, be added 1mol/L HCl impregnate for 24 hours with
Remove not wrapped Fe3O4Particle is filtered, is alternately washed 4 times with distilled water and dehydrated alcohol, until pH=7,60 DEG C of vacuum
Lower dry 12h obtains the magnetic graphene polystyrene complex microsphere sewage-treating agent.
Embodiment 2
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent, preparation step are as follows:
A), chemical precipitation method prepares nanometer Fe3O4Particle: under nitrogen protection, by 16.2 parts of FeCl3With 12.7 parts of FeCl2
It is added in 1000L deionized water, the sodium hydroxide solution that concentration is 1mol/L is instilled while stirring at 30 DEG C, until pH value
Stop reaction when close to 11；Then 60 DEG C of stirring curing 1h are warming up to, are stood after stopping stirring, with NdFeB magnetic filter point
Separate out Fe3O4, with alternately washing 5 times of distilled water and dehydrated alcohol, until pH=7, dry 12h at 60 DEG C of vacuum is obtained described
Nanometer Fe3O4Particle；
B), nanometer Fe3O4Magnetic current is modifies: in the container equipped with 250.0 parts of ethyl alcohol, 23.0 parts of nanometer Fes are added3O4
Particle and 35.0 parts of polyethylene glycol, are warming up at 60 DEG C and quickly stir 3h, the stratification 4h under high-intensity magnetic field, remove upper liquid
Then 230.0 parts of deionized waters are added in body, disperse 15min with ultrasonic wave, then mechanical stirring is for 24 hours, obtains modified Fe3O4Water
Based magnetofluid；
C), magnetic oxygenated graphene complex microsphere is prepared: in four mouthfuls of reactions equipped with thermometer, blender and condenser pipe
In device, under nitrogen protection, be added 50.0 parts of ethyl alcohol and 30.0 parts of deionized waters and 2.6 parts of PVP, stirring to dissolving, then according to
0.3 part of initiator A IBN of secondary addition, 25.0 parts of styrene, 4.0 parts of itaconic acids, 6.0 parts of MODIFIED Fes3O4Magnetic fluid and 4.0 parts of oxygen
Graphite alkene after being stirred until homogeneous, stands 3h after ultrasonic wave dispersion 10min；It starts and stirs and to be warming up to 70 DEG C of holding constant temperature anti-
7h is answered, then is warming up to 85 DEG C of reaction 1h；Product NdFeB filter is separated, the HCl that 1mol/L is added impregnates for 24 hours to remove
Not wrapped Fe3O4Particle is filtered, is alternately washed 4 times with distilled water and dehydrated alcohol, up at pH=7,60 DEG C of vacuum
Dry 12h, obtains the magnetic graphene polystyrene complex microsphere sewage-treating agent.
Embodiment 3
A kind of magnetic graphene polystyrene complex microsphere sewage-treating agent, preparation step are as follows:
A), chemical precipitation method prepares nanometer Fe3O4Particle: under nitrogen protection, by 16.2 parts of FeCl3With 12.7 parts of FeCl2
It is added in 1000L deionized water, the sodium hydroxide solution that concentration is 1mol/L is instilled while stirring at 30 DEG C, until pH value
Stop reaction when close to 11；Then 60 DEG C of stirring curing 1h are warming up to, are stood after stopping stirring, with NdFeB magnetic filter point
Separate out Fe3O4, with alternately washing 5 times of distilled water and dehydrated alcohol, until pH=7, dry 12h at 60 DEG C of vacuum is obtained described
Nanometer Fe3O4Particle；
B), nanometer Fe3O4Magnetic current is modifies: in the container equipped with 300.0 parts of ethyl alcohol, 25.0 parts of nanometer Fes are added3O4
Particle and 45.0 parts of polyethylene glycol, are warming up at 60 DEG C and quickly stir 3h, the stratification 5h under high-intensity magnetic field, remove upper liquid
Then 250.0 parts of deionized waters are added in body, disperse 15min with ultrasonic wave, then mechanical stirring is for 24 hours, obtains modified Fe3O4Water
Based magnetofluid；
C), magnetic oxygenated graphene complex microsphere is prepared: in four mouthfuls of reactions equipped with thermometer, blender and condenser pipe
In device, under nitrogen protection, be added 60.0 parts of ethyl alcohol and 35.0 parts of deionized waters and 3.2 parts of PVP, stirring to dissolving, then according to
0.4 part of initiator A IBN of secondary addition, 30.0 parts of styrene, 4.5 parts of N, N '-methylene-bisacrylamide, 8.0 parts of MODIFIED Fes3O4
Magnetic fluid and 5.0 parts of graphene oxides after being stirred until homogeneous, stand 3h after ultrasonic wave dispersion 10min；It starts stirring and heats up
To 70 DEG C of holding isothermal reaction 8h, then it is warming up to 85 DEG C of reaction 1h；Product NdFeB filter is separated, is added 1mol/L's
HCl impregnates for 24 hours to remove not wrapped Fe3O4Particle is filtered, is alternately washed 5 times with distilled water and dehydrated alcohol, until
PH=7, dry 12h, obtains the magnetic graphene polystyrene complex microsphere sewage-treating agent at 60 DEG C of vacuum.
It is heavy metal ion adsorbed measure examination: on the market magnetic polystyrene microsphere inorganic agent (comparative example 1) and magnetism
Graphene oxide inorganic agent (comparative example 2) and the embodiment of the present invention carry out heavy metal ion adsorbed amount contrast test；Identical
Under the conditions of, take 0.05g institute test specimens to be placed in the Pb containing 50mL 200mg/L respectively2+Solion, the Cr containing 150mg/L6 +Solion, the Cu containing 100mg/L2+Solion and Hg containing 100mg/L2+In solion, stirring is adsorbed,
Using each concentration of heavy metal ion in solution after atomic spectrophotometer test absorption, the heavy metal ion adsorbed amount of each sample
Data are as shown in table 1:
1 the embodiment of the present invention of table and comparative example are to various heavy metal ion adsorbed amounts (mg/g)
| Inorganic agent | Pb2+Adsorbance | Cr6+Adsorbance | Cu2+Adsorbance | Hg2+Adsorbance |
| Embodiment 1 | 182.5 | 136.4 | 93.2 | 92.5 |
| Embodiment 2 | 186.2 | 137.2 | 96.6 | 94.8 |
| Embodiment 3 | 187.6 | 138.5 | 97.4 | 95.6 |
| Comparative example 1 | 165.7 | 126.5 | 76.2 | 78.2 |
| Comparative example 2 | 158.4 | 122.8 | 65.2 | 68.5 |
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Art technology
Personnel should be appreciated that invention scope involved in the application, however it is not limited to skill made of the specific combination of above-mentioned technical characteristic
Art scheme, while should also cover in the case where not departing from the inventive concept, by above-mentioned technical characteristic or its equivalent feature into
Row any combination and the other technical solutions formed.Such as features described above and (but being not limited to) disclosed herein have class
Technical characteristic like function is replaced mutually and the technical solution that is formed.
Claims (6)
1. a kind of preparation method of magnetic graphene polystyrene complex microsphere sewage-treating agent, it is characterised in that: the system
Preparation Method, preparation step are as follows:
A), chemical precipitation method prepares nanometer Fe3O4Particle: under nitrogen protection, the FeCl for being 0.1mol/L by concentration3And concentration
For the FeCl of 0.1mol/L21:1 is added in reactor solution in molar ratio, is instilled concentration while stirring at 30 DEG C and is
The sodium hydroxide solution of 1mol/L, until stopping reaction when pH value is close to 11；Then 60 DEG C of stirring curing 1h are warming up to, stop stirring
It is stood after mixing, isolates Fe with NdFeB magnetic filter3O4, alternately washed 4~6 times with distilled water and dehydrated alcohol, until pH
=7, dry 12h, obtains the nanometer Fe at 60 DEG C of vacuum3O4Particle；
B), nanometer Fe3O4Magnetic current is modifies: in the container equipped with 200.0~300.0 parts of ethyl alcohol, being added 20.0~25.0 parts and receives
Rice Fe3O4Particle and 30.0~45.0 parts of polyethylene glycol, are warming up at 60 DEG C and quickly stir 3h, under high-intensity magnetic field stratification 3~
5h removes supernatant liquid, and 200.0~250.0 parts of deionized waters are then added, and disperses 15min, then mechanical stirring with ultrasonic wave
For 24 hours, modified Fe is obtained3O4Water-based magnetic fluid；
C), magnetic oxygenated graphene complex microsphere is prepared: in four mouthfuls of reactors equipped with thermometer, blender and condenser pipe,
Under nitrogen protection, 30.0~60.0 parts of ethyl alcohol and 25.0~40.0 parts of deionized waters and 0.5~3.5 part of dispersing agent is added, stirs
It mixes to dissolution, then sequentially adds that 0.1~0.4 part of initiator A IBN, 15.0~30.0 parts of styrene, 1.0~5.0 parts containing carboxyl
Monomer, 3.0~10.0 parts of MODIFIED Fes3O4Magnetic fluid and 2.0~5.0 parts of graphene oxides, after being stirred until homogeneous, ultrasonic wavelength-division
2~4h is stood after dissipating 5~10min；It starts and stirs and be warming up to 70 DEG C of holding 6~8h of isothermal reaction, then be warming up to 85 DEG C of reactions
1h；Product NdFeB filter is separated, the HCl that 1mol/L is added impregnates for 24 hours to remove not wrapped Fe3O4Particle is taken out
Filter obtains the magnetism up to 12h dry at pH=7,60 DEG C of vacuum with distilled water and dehydrated alcohol alternately washing 3~5 times
Graphene polystyrene complex microsphere sewage-treating agent.
2. preparation method according to claim 1, it is characterised in that: the carboxylic monomer is acrylic acid, methyl-prop
Olefin(e) acid, itaconic acid, maleic anhydride, N, at least one of N '-methylene-bisacrylamide.
3. preparation method according to claim 1, it is characterised in that: the dispersing agent is polyvinylpyrrolidone, alkyl
At least one of phenol polyethenoxy ether, polyethylene glycol, polyacrylic acid, polyvinyl alcohol.
4. preparation method according to claim 1, it is characterised in that: the dispersing agent is polyvinylpyrrolidone.
5. preparation method according to claim 1, it is characterised in that: the graphene oxide by Hum mers method,
Staudenmaier method, electrochemical process or the preparation of Brodie method.
6. preparation method according to claim 1, it is characterised in that: the graphene oxide is the preparation of Hum mers method.
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| CN111229167A (en) * | 2020-01-20 | 2020-06-05 | 华南理工大学 | Thiosemicarbazide modified magnetic graphene oxide adsorbent and preparation method and application thereof |
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Application publication date: 20190517 |