CN104258827B - Magnetic mesoporous carbon of Polyaniline-modified and its preparation method and application - Google Patents
Magnetic mesoporous carbon of Polyaniline-modified and its preparation method and application Download PDFInfo
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- CN104258827B CN104258827B CN201410474205.3A CN201410474205A CN104258827B CN 104258827 B CN104258827 B CN 104258827B CN 201410474205 A CN201410474205 A CN 201410474205A CN 104258827 B CN104258827 B CN 104258827B
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses magnetic mesoporous carbon of a kind of Polyaniline-modified and its preparation method and application, wherein the magnetic mesoporous carbon of Polyaniline-modified makes polyaniline adsorb on the surface of magnetic mesoporous silicon by the oxidation polymerization effect of aniline, and magnetic mesoporous silicon includes mesoporous carbon and magnetic composite.Its preparation method specifically includes following steps: joined by aniline in hydrochloric acid, is slowly added into magnetic mesoporous carbon by mechanical agitation and obtains magnetic mesoporous carbon complex；Being joined by magnetic mesoporous carbon complex in the mixed solution of Ammonium persulfate. and aniline, under conditions of ice bath, continuously stirred 10～12 h obtain the magnetic mesoporous carbon of Polyaniline-modified.The magnetic mesoporous carbon of this Polyaniline-modified can be used for heavy metal ion in adsorbent solution, and after having adsorbed, available Magnet separates.The magnetic mesoporous carbon preparation technology of the Polyaniline-modified of the present invention is simple, and adsorbent magnetic property is stable, has environmental protection, adsorption capacity is big, equilibration time is short and the advantage such as applied widely.
Description
Technical field
The present invention relates to technical field of mesoporous materials, magnetic mesoporous carbon particularly relating to a kind of Polyaniline-modified and preparation method thereof and the application at removal Heavy Metals in Waters ion.
Background technology
Heavy metal pollution is widely present in various industrial wastewater, and publilc health and ecological environment are caused serious harm.Just because of this, heavy metal pollution is controlled of great interest.The method of the heavy metal in existing removing waste water, mainly has: chemical precipitation or flocculence, membrane technology, electroreduction, ion exchange and absorption method.Wherein, absorption method is convenient with its adsorption operations, and the wide variety of adsorbent, flexible design, regenerating easily, waste water that is efficient and that process are suitable to recycle and be widely used.Owing to magnetic adsorbent can realize the sharp separation with liquid phase under the effect of external magnet, can avoid centrifugal or filter the inconvenience that lock out operation brings, thus polluting process field at heavy metal wastewater thereby and obtain concern greatly.Giving the absorption property that adsorbent can improve adsorbent with magnetic and porous, the existence of porous increases the specific surface area of adsorbent, reduces the diffusional resistance of solute, is beneficial to be rapidly achieved adsorption equilibrium.Meanwhile, modify, by surface, functional groups such as making amino, carboxyl, hydroxyl, sulfydryl on adsorbent band to chelate or complexation heavy metal ion is also the important channel improving absorption property.But, in prior art, surface is modified the adsorbent of the functional groups such as amino, carboxyl, hydroxyl, sulfydryl and is all only existed simple absorption property, and adsorption effect still can not meet the requirement of present stage heavy metal containing wastewater treatment, needs a kind of more efficient adsorbent of searching badly.
Polyaniline is a kind of high molecular weight water soluble polymer, and its strand has substantial amounts of amido atom N, and heavy metal has the strongest sequestering power.This characteristic has caused the extensive concern of Chinese scholars, and has been applied to numerous research field.But due to the water miscible feature of polyaniline, it is difficult to ensure that it is in the operability of absorption heavy metal ions in wastewater.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that the magnetic mesoporous carbon of the Polyaniline-modified that a kind of magnetic property is stable, suitable environment is wide；Additionally provide a kind of technique simple and be suitable to the preparation method of magnetic mesoporous carbon of Polyaniline-modified of large-scale production；Additionally provide the application process of heavy metal ion in the magnetic mesoporous carbon adsorbent solution of the Polyaniline-modified that a kind of adsorption capacity is big, adsorption efficiency is high, time of equilibrium adsorption is short.
For solving above-mentioned technical problem, the invention provides the magnetic mesoporous carbon of a kind of Polyaniline-modified, make polyaniline absorption obtain the magnetic mesoporous carbon of Polyaniline-modified on the surface of magnetic mesoporous carbon by the oxidation polymerization effect of aniline.
Further, magnetic mesoporous carbon being loaded with magnetic composite, magnetic composite is preferably iron oxides.
Further, the aperture of the magnetic mesoporous carbon of aforementioned Polyaniline-modified is 5 nm～8 nm.
As total technology design, present invention also offers above-mentioned magnetic mesoporous carbon preparation method based on Polyaniline-modified, comprise the following steps:
S1, by aniline and mixed in hydrochloric acid, be then slowly added into magnetic mesoporous carbon by mechanical agitation and obtain magnetic mesoporous carbon complex；
S2, being joined by aforementioned magnetic mesoporous carbon complex in the mixed solution of Ammonium persulfate. and aniline, under conditions of ice bath, continuously stirred 10～12 h obtain the magnetic mesoporous carbon of Polyaniline-modified.
Further, aforementioned preparation process also includes post-processing step: the magnetic mesoporous carbon of aforementioned Polyaniline-modified is passed through Magnetic Isolation, carry out ultra-pure water cleaning, ethanol purge respectively, more under vacuo to be dried to obtain the magnetic mesoporous carbon sterling of aforementioned Polyaniline-modified at 50 DEG C～60 DEG C.
Further, aforementioned magnetic mesoporous carbon is prepared by following steps: be impregnated in alcohol blend by mesoporous silicon SBA-15,10 h～12 h are heated in the air of 90 DEG C～100 DEG C, then obtaining magnetic mesoporous carbon with 900 DEG C～1000 DEG C calcining 1 h～2 h under the atmosphere of nitrogen, aforementioned alcohol blend uses and the nine water ferric nitrates of 0.07～0.08 g/mL and the oxalic acid of 0.003～0.006 g/mL is dissolved in ethanol and being prepared.
Further, aforementioned mesoporous silicon SBA-15 and nine liquid glauber salt acid weight of iron ratios are 1: 0.35～0.8, and the mass ratio of aforementioned mesoporous silicon and oxalic acid is 1: 0.015～0.06.
Further, in abovementioned steps S2, the mixed solution of aforementioned Ammonium persulfate. and aniline is dissolved in the hydrochloric acid that concentration is 0.1 M～0.3 M by the Ammonium persulfate. that mol ratio is 1: 1～1.2 and aniline and preparing.
As total technology design, the magnetic mesoporous carbon or the aforementioned preparation process that present invention also offers aforementioned Polyaniline-modified prepare the application in heavy-metal ion removal of the magnetic mesoporous carbon of Polyaniline-modified.
Further, aforementioned applications method specifically includes following steps: is joined by the magnetic mesoporous carbon of aforementioned Polyaniline-modified in the solution containing heavy metal ion and carries out concussion absorption 3 more than h, then carries out Magnetic Isolation, complete absorption.
Further, the addition of aforementioned magnetic mesoporous carbon adsorbent is 1 g/L～2 g/L,；In the aforementioned solution containing heavy metal ion, the concentration of heavy metal ion is 50 mg/L～500
Mg/L, pH value is 1.5～2.5.
Compared with prior art, it is an advantage of the current invention that:
(1) present invention uses magnetic mesoporous carbon to be united by the chemical interaction of the polyaniline chain between amido or imido grpup and magnetic mesoporous carbon surface as the main carriers of adsorbent, polyaniline.Owing to magnetic mesoporous carbon is porous structure, there is great specific surface area, polyaniline adsorbs at magnetic mesoporous carbon surface, be conducive to the heavy metal ion in Rapid contact waste water, shorten the time required for adsorption equilibrium greatly, improve the adsorption capacity of the magnetic mesoporous carbon of Polyaniline-modified, present huge absorption property.
(2) present invention uses mesoporous carbon as absorption carrier, when polyaniline adsorbs in mesoporous carbon, stability can be kept in strong acid and strong base environment, compared to the mesoporous silicon of Polyaniline-modified, improve the mechanically stable ability of the magnetic mesoporous carbon of Polyaniline-modified, suitable environment is wider.Applicants experimentally found that, by the mesoporous silicon of Polyaniline-modified and the mesoporous carbon of Polyaniline-modified, waste water is processed respectively, regulation pH is 2～9, the clearance of the magnetic mesoporous silicon of Polyaniline-modified is down to 50% from 95%, and the removal efficiency of the magnetic mesoporous carbon of Polyaniline-modified is down to 60% from 93%, it can be seen that, in the case of degradation effect is almost consistent, mesoporous carbon is more stable as the adsorbent effect of carrier, and suitable environment is wider.
(3) present invention supported ferriferous oxide in mesoporous carbon, owing to iron oxides has paramagnetism, under the effect of external magnetic field, the easily separation of high efficiency, low cost from liquid phase, simple to operate, be applicable to large-scale waste water process.
(4) preparation method of the magnetic mesoporous carbon of the Polyaniline-modified of the present invention, technique is simple and is suitable to large-scale production.
(5) present invention magnetic mesoporous carbon application process of heavy metal ion in adsorbent solution of Polyaniline-modified, adsorption capacity is big, adsorption efficiency is high, time of equilibrium adsorption is short, adsorbent environmental protection, can be widely used in the process of heavy metal wastewater thereby.
Accompanying drawing explanation
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete description.
Fig. 1 is the transmission electron microscope picture of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1.
Fig. 2 is the infrared spectrum schematic diagram of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1.
Fig. 3 is the nitrogen adsorption-desorption isotherm figure of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1.
Fig. 4 is the graph of pore diameter distribution of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1.
Fig. 5 is adsorbance and the relation schematic diagram of the initial concentration of heavy metal ion in solution of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1.
Fig. 6 is the relation schematic diagram that the surplus after the Adsorption of Heavy Metals solution of the magnetic mesoporous carbon of the Polyaniline-modified of the embodiment of the present invention 1 changes with adsorption time.
Fig. 7 is the heavy metal adsorption amount relation schematic diagram with pH value of solution of the magnetic mesoporous carbon of the Polyaniline-modified of the present invention.
Detailed description of the invention
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but protection domain not thereby limiting the invention.
Embodiment
Material and instrument employed in following example are commercially available；Wherein mesoporous silicon SBA-15 uses hydrothermal synthesis method to prepare.
Embodiment
1
:
The preparation method of the magnetic mesoporous carbon of a kind of Polyaniline-modified, specifically includes following steps:
(1) magnetic mesoporous carbon is prepared: the content taking 1.0 g mesoporous silicon SBA-15(mesoporous silicons can also is that 1.0～2.0g) it is impregnated in the ethanol mixed solution of 10 mL that (alcohol blend uses the nine water ferric nitrates and 0.05 of 0.721 g
The oxalic acid of g is dissolved in the ethanol that volume is 10 mL and preparing, and in the present invention, the concentration of nine water ferric nitrates is 0.07～0.08 g/mL, the concentration of oxalic acid is 0.003～0.006 g/mL, all can reach same or analogous technique effect).Then, 2.0 it are added dropwise over
(content of furfuryl alcohol is at 2.0 mL～3.0 for the furfuryl alcohol of mL
ML all can implement) obtain mixture.Aforesaid mixture heats in the air of 90 DEG C 10 h(in the air of 90 DEG C～100 DEG C, heat 10 h～12 h all can reach same or analogous technique effect), then under the atmosphere of nitrogen, all can reach same or analogous technique effect with 900 DEG C of calcining 2 h(with 900 DEG C～1000 DEG C calcining 1 h～2 h) obtain calcined product.Finally, aforesaid calcined product is placed in the sodium hydroxide solution (naoh concentration is 2.0 M) that temperature is 90 DEG C, through 0.2 μm membrane filtration, with washes of absolute alcohol, is dried to obtain magnetic mesoporous carbon with 60 DEG C.
In the preparation process of above-mentioned magnetic mesoporous carbon, mesoporous silicon SBA-15 and nine liquid glauber salt acid weight of iron ratios can also be 1: 0.35～0.8, and the mass ratio of mesoporous silicon and oxalic acid can also be 1: 0.015～0.06, all can reach same or analogous technique effect.
(2) magnetic mesoporous carbon of Polyaniline-modified is prepared:
S1, the aniline of 2.0 mL is joined 400
ML concentration is in the hydrochloric acid of 0.2 M, is then slowly added into, by mechanical agitation, the magnetic mesoporous carbon that the step (1) of 1.0 g prepares and obtains magnetic mesoporous carbon complex；
S2, being joined by aforementioned magnetic mesoporous carbon complex in the mixed solution of 200 mL Ammonium persulfate .s and aniline, under conditions of ice bath, continuously stirred 12 h obtain the magnetic mesoporous carbon of Polyaniline-modified；
S3, then taking solid by Magnetic Isolation, with ultra-pure water and ethanol purge, then (be dried with 50 DEG C～60 DEG C and all can implement) is dried to obtain the magnetic mesoporous carbon sterling of Polyaniline-modified at 60 DEG C under vacuo.
In embodiment 1, the mixed solution of ammonium sulfate and aniline is dissolved in the hydrochloric acid that concentration is 0.2 M by the Ammonium persulfate. that mol ratio is 1: 1 and aniline and preparing；The mol ratio of Ammonium persulfate. and aniline solution is 1: 1～1.2, and the concentration of hydrochloric acid is 0.1 M～0.3 M, all can reach same or analogous technique effect.
The magnetic mesoporous carbon of the Polyaniline-modified that embodiment 1 prepares, makes polyaniline absorption be loaded with magnetic composite on the surface of magnetic mesoporous carbon, aforementioned magnetic mesoporous carbon by the oxidation polymerization effect of aniline.Magnetic composite is iron oxides in the present invention.
The magnetic mesoporous carbon of Polyaniline-modified embodiment 1 prepared carries out transmission electron microscopy, and Fig. 1 is the transmission electron microscope picture of the magnetic mesoporous carbon of Polyaniline-modified, and as shown in Figure 1, the duct of the magnetic mesoporous carbon of this Polyaniline-modified is regular, is evenly distributed.
The magnetic mesoporous carbon of Polyaniline-modified is carried out respectively infrared spectrum analysis, as can be known from Fig. 2, the strong absworption peak 3560 in infrared spectrum
Cm, 1302 cm, 1140 and 567cm are respectively functional group's N-H stretching vibration peak, C-H stretching vibration peak, C-H scissoring vibration peak and Fe-O stretching vibration peak；The absworption peak being in 1475cm and 1592 cm is C=C stretching vibration peak, and the appearance of N-H stretching vibration peak causes mainly due to polyaniline.
See Fig. 3, the magnetic mesoporous carbon of Polyaniline-modified is carried out the experiment of nitrogen adsorption and desorption, obtains a hysteretic loop structure significantly, it follows that the magnetic mesoporous carbon of Polyaniline-modified still keeps meso-hole structure.
See Fig. 4, the magnetic mesoporous carbon of Polyaniline-modified is carried out pore analysis, it is possible to find the aperture integrated distribution of the magnetic mesoporous carbon of Polyaniline-modified is at 5nm～8nm.
The application in heavy-metal ion removal of the magnetic mesoporous carbon of Polyaniline-modified:
It is respectively adopted the different initial concentration of hexavalent chromium, different sorption reaction times or the pH value of different solutions, tests the ability of the magnetic mesoporous carbon of the above-mentioned Polyaniline-modified heavy metal ion in adsorbent solution, specifically comprise the following steps that
(1) pH preparing 10 group of 10 mL is the solution containing hexavalent chromium of 2.0, and in regulation solution, the initial concentration of chromium ion is 10 respectively
mg/L、20 mg/L、50
mg/L、80 mg/L、100
mg/L、200 mg/L、300
Mg/L, 400 mg/L and 500
Mg/L, is separately added into the magnetic mesoporous carbon of the Polyaniline-modified of 0.01 g embodiment 1, at room temperature, with concussion absorption 3 h under 150 rpm speed conditions.Sampling, with after the magnetic porous adsorbent of Magnet heavy metal ion by preceding adsorption and solution separating 3 min, completes absorption.
Solution ultraviolet-uisible spectrophotometer after separating is measured and calculates.Result is as it is shown in figure 5, as shown in Figure 5: the equilibrium adsorption capacity of adsorbent along with in solution the initial concentration of hexavalent chromium increase and increase, when initial concentration reaches 300 mg/L, adsorbance is basically unchanged.In above-mentioned application process, the addition of the magnetic mesoporous carbon of Polyaniline-modified all can reach same or analogous technique effect at 0.01 ~ 0.02 g.
(2) solution containing hexavalent chromium that 11 group of 10 mL concentration is 80 mg/L is prepared, it is separately added into the magnetic mesoporous carbon of the Polyaniline-modified of 0.01 g embodiment 1, regulation pH value is 2, adsorption reaction is carried out under room temperature and 150 rpm speed conditions, it is 2 min respectively at the response time, samples when 5 min, 10 min, 20 min, 30 min, 40 min and 60 min, 90 min, 120min, 180 min, after Magnetic Isolation 3 min, it is measured and calculates.
As shown in Figure 6, it will be appreciated from fig. 6 that the magnetic porous adsorbent of the present invention is shorter to the time of equilibrium adsorption of zinc ion, 60 min i.e. can reach saturated absorption to result.In above-mentioned application process, the addition of the magnetic mesoporous carbon of Polyaniline-modified is 0.01 ~ 0.02
G all can reach same or analogous technique effect.
(3) prepare 5 groups of 10mL concentration be 80 mg/L containing chromium ion solution, and regulation pH value is 2,3,5,7,9 respectively, the magnetic porous adsorbent of 0.01 g embodiment 1 is added in often group is containing chromium ion solution, 3 h are shaken under room temperature and 150 rpm speed conditions, sampling, after Magnetic Isolation 3 min, ultraviolet-uisible spectrophotometer is utilized to measure the amount of heavy metal not to be adsorbed in solution.
As it is shown in fig. 7, as shown in Figure 7, the adsorption efficiency of the magnetic mesoporous carbon of the Polyaniline-modified of the present invention reduces experimental result along with the rising of pH, thus, for keeping its optimal adsorption effect, pH is set to 2.0 optimal.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction.Although the present invention discloses as above with preferred embodiment, but is not limited to the present invention.Any those of ordinary skill in the art, in the case of without departing from the spirit of the present invention and technical scheme, technical solution of the present invention is made many possible variations and modification by the method and the technology contents that all may utilize the disclosure above, or is revised as the Equivalent embodiments of equivalent variations.Therefore, every content without departing from technical solution of the present invention, to any simple modification made for any of the above embodiments, equivalent, equivalence change and modify according to the technical spirit of the present invention, all still fall within the range of technical solution of the present invention protection.
Claims (10)
1. the magnetic mesoporous carbon of a Polyaniline-modified, it is characterised in that make polyaniline absorption obtain the magnetic mesoporous carbon of Polyaniline-modified on the surface of magnetic mesoporous carbon by the oxidation polymerization effect of aniline；The preparation method of the magnetic mesoporous carbon of described Polyaniline-modified, comprises the following steps:
S1, by aniline and mixed in hydrochloric acid, be then slowly added in magnetic mesoporous carbon by mechanical agitation and obtain magnetic mesoporous carbon complex；
S2, described magnetic mesoporous carbon complex is joined in the mixed solution of Ammonium persulfate. and aniline, the continuously stirred magnetic mesoporous carbon obtaining Polyaniline-modified under conditions of ice bath.
Magnetic mesoporous carbon the most according to claim 1, it is characterised in that be loaded with magnetic composite on described magnetic mesoporous carbon, described magnetic composite is iron oxides, and the aperture of the magnetic mesoporous carbon of described Polyaniline-modified is 5 nm～8 nm.
3. the preparation method of the magnetic mesoporous carbon of the Polyaniline-modified described in a claim 1 or 2, it is characterised in that comprise the following steps:
S1, by aniline and mixed in hydrochloric acid, be then slowly added in magnetic mesoporous carbon by mechanical agitation and obtain magnetic mesoporous carbon complex；
S2, described magnetic mesoporous carbon complex is joined in the mixed solution of Ammonium persulfate. and aniline, the continuously stirred magnetic mesoporous carbon obtaining Polyaniline-modified under conditions of ice bath.
Preparation method the most according to claim 3, it is characterized in that, described preparation method also includes post-processing step: the magnetic mesoporous carbon of described Polyaniline-modified is passed through Magnetic Isolation, carry out ultra-pure water cleaning, ethanol purge respectively, more under vacuo with 50 DEG C～the 60 DEG C magnetic mesoporous carbon sterlings being dried to obtain Polyaniline-modified.
5. according to the preparation method described in claim 3 or 4, it is characterized in that, described magnetic mesoporous carbon is prepared by following steps: be impregnated in alcohol blend by mesoporous silicon SBA-15,10 h～12 h are heated in the air of 90 DEG C～100 DEG C, then obtaining magnetic mesoporous carbon with 900 DEG C～1000 DEG C calcining 1 h～2 h under the atmosphere of nitrogen, described alcohol blend uses and the nine water ferric nitrates of 0.04～0.8 g/mL and the oxalic acid of 0.003～0.006 g/mL is dissolved in ethanol and being prepared.
Preparation method the most according to claim 5, it is characterised in that described mesoporous silicon SBA-15 and nine liquid glauber salt acid weight of iron ratios are 1: 0.35～0.8, and the mass ratio of described mesoporous silicon and oxalic acid is 1: 0.015～0.06.
7. according to the preparation method described in claim 3 or 4, it is characterised in that the mixed solution of Ammonium persulfate. described in described step S2 and aniline is dissolved in the hydrochloric acid that concentration is 0.1 M～0.3 M by the Ammonium persulfate. that mol ratio is 1: 1～1.2 and aniline and preparing.
8. preparation method described in the magnetic mesoporous carbon of a Polyaniline-modified as claimed in claim 1 or 2 or any one of claim 3 to 7 prepares the application in heavy-metal ion removal of the magnetic mesoporous carbon of Polyaniline-modified.
Application the most according to claim 8, it is characterised in that comprise the following steps: the magnetic mesoporous carbon of described Polyaniline-modified is joined in the solution containing heavy metal ion and carry out concussion absorption 3 more than h, then carry out Magnetic Isolation, complete absorption.
Application the most according to claim 9, it is characterised in that the addition of the magnetic mesoporous carbon of described Polyaniline-modified is 1 g/L～2 g/L；In the described solution containing heavy metal ion, the concentration of heavy metal ion is 50 mg/L～500 mg/L, and pH value is 1.5～2.5.
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| CN111495367B (en) * | 2020-06-01 | 2023-02-24 | 西安科技大学 | Magnetic polyaniline-porous carbon-Fe 3 O 4 Preparation method and application of photo-Fenton catalyst |
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