Beruflich Dokumente
Kultur Dokumente
a r t i c l e i n f o a b s t r a c t
Article history: Magnetic photocatalyst iodine and nitrogen codoped TiO2 based on chitosan decorated magnetic
Received 29 June 2016 activated carbon (I-N-T/CMAC) was prepared via simple coprecipitation and sol-gel method. The char-
Received in revised form 2 August 2016 acteristics of photocatalysts were investigated by X-ray diffraction (XRD), N2 adsorptiondesorption
Accepted 6 August 2016
isotherm, eld emission scanning electron microscopy (FESEM), energy dispersive spectrometry (EDS),
Available online 9 August 2016
fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), UVvis diffuse reection
spectroscopy (UVvis DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetome-
Keywords:
ter (VSM). It turned out that the prepared material had large surface area, enhanced absorption of visible
Magnetic photocatalyst
Activated carbon
light, and magnetically separable properties when mole ratio of I/Ti was 0.1. Iodine-nitrogen codoped
Codoped magnetic photocatalyst was used for the removal of salicylic acid (SA), and the rate of adsorption reaction
Water treatment for SA by I0.1 -N-T/CMAC followed the pseudo second-order kinetic. Under visible light irradiation, 89.71%
Reusability SA with initial concentration = 30 mg/L could be removed by I0.1 -N-T/CMAC, and photodegradation rate
of SA on I0.1 -N-T/CMAC composites was 0.0084 min1 which is about 4 times higher than that of magnetic
photocatalyst with nitrogen doped only. The effects of SA initial concentration, pH, coexisting anions and
humic acid to the degradation of SA with the prepared material were also investigated. Main oxidative
species in the photodegradation process are OH and h+ .
2016 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2016.08.040
0169-4332/ 2016 Elsevier B.V. All rights reserved.
X. Wang et al. / Applied Surface Science 390 (2016) 190201 191
2. Experimental
Fig. 3. The SEM images and element maps: AC(a), low and high magnication images for I0.1 -N-T/CMAC (bd), element maps images for I0.1 -N-T/CMAC (eh), respectively.
X. Wang et al. / Applied Surface Science 390 (2016) 190201 193
Table 1
Effects of mole ratios of I/Ti on specic surface area, crystal size and band gap of Ix -N-T/CMAC .
Photocatalyst Specic surface area (m2 g1 ) Average Pore size (nm) Total pore volume (cm3 g1 ) Crystal size(nm) Eg /eV
Table 2
Surface atomic concentrations of catalysts from XPS analyses.
Ti O N C I
Table 3
Room temperature magnetic properties for synthesized Fe3 O4 , N-T/CMAC and I0.1 -
N-T/CMAC respectively.
brated by C 1s level from carbon samples at 284.6 eV, and the high
resolution XPS peaks were tted with mixed Lorentzian-Gaussian
curves after a Linear background subtraction. Optical property Fig. 4. FTIR spectra of N-T/CMAC and I0.1 -N-T/CMAC.
was obtained in the range of 200700 nm on a Shimadzu UV2550
UVvis-spectrophotometer with BaSO4 as a reectance standard.
tor. There was a cooling device to eliminate thermal effect and a
Photoluminescence (PL) spectra were measured at room temper-
tube to supply air (0.1 L/min). During the photocatalytic reaction,
ature on a Steady state/Lifetime Fluorescence Spectrophotometer
5 mL solution were sampled and ltered with 0.45 m membrane
(QM-40, PTI, USA). Nitrogen adsorption and desorption isotherms
lter at each time intervals for analysis. The concentration of
were carried out using an ASAP 2020, Micrometritics analyzer to
SA was detected by a Shimadzu UV-2700 spectrophotometer at
obtain Brunauer-Emmett-Teller (BET) surface area. Magnetic prop-
295 nm which corresponds to the characteristic absorption peak
erties (M-H curve) were collected at room temperature by using a
of SA.
vibrating sample magnetometer (VSM).
Fig. 5. XPS survey spectra of I0.1 -N-T/CMAC: (a) Ti 2p (b):N 1s, (c): C 1s, (d): I 3d.
tions may lead to the formation of this impurity phase. Moreover, ity of materials [16,26]. In this way, the mole ratio of I/Ti = 0.1
the rst small peak at 2 = 23.6 could assign to the existence of is suitable to get higher specic surface area and photocatalytic
few graphite which was from activated carbon [34,35]. When the activity.
mole ratio of I/Ti is 0.1, the sample own the smallest crystallite size The morphologies of AC and I0.1 -N-T/CMAC composites are
and the photocatalyst could disperse much better than the other shown in Fig. 3. Comparing Fig. 3(a) and (b), it can be seen that
samples, and hence the peak at 2 = 23.6 was weakened which nanometer-scale TiO2 particles were well dispersed on the surface
indicated MAC was coated much better. of AC. Furthermore, as shown in Fig. 3(c) and (d), the surface of AC
Consequently, nitrogen adsorption-desorption isotherms of Ix - was covered by the agglomerates of many irregular size TiO2 crys-
N-T/CMAC samples are shown in Fig. 2. To all the samples, type IV tallites. Element maps (Fig. 3(e)(h)) show the coexistence of large
isotherms are detected, which indicate the presence of mesoporous amount titanium, oxygen and iodine on the surface of composites.
structure [1]. The average pore diameters of the samples (Table 1) The distribution of Ti, O and I was similar, suggesting that TiO2
were 5.6176.313 nm, also conrmed the existence of mesoporous particles were well-dispersed on the support. Moreover, the mor-
structure. The pore channel allow light to scatter inside, and the phology of I0.1 -N-T/CMAC sample was observed by TEM (Fig. S1),
absorption of light can be enhanced [36]. I0.05 -N-T/CMAC and I0.1 - which also indicated that the coated particle consisted of irregular-
N-T/CMAC have the higher specic surface area than N-T/CMAC, shape nanoparticles.
which is 199.71 and 199.3 m2 g1 respectively. Further, Increas- Fig. 4 shows FTIR spectrum of N-T/CMAC and I0.1 -N-T/CMAC.
ing the mole ratio of I/Ti to 0.15 reduce the specic surface area The bands at about 3415 cm1 and 1635 cm1 could be assigned
to 162.09 m2 g1 . Meanwhile the average pore size and total pore to the stretching vibrations of OH groups from hydroxyls and
volume decreased as the increase of potassium iodate addition the exural vibrations of H O H groups adsorbed on the sur-
amount. Excess potassium iodate may block the micropores of Ix - face and channel of TiO2 materials[37,38]. The peaks at 1529 cm1 ,
N-T/CMAC. While the micropores nanostructure and larger specic 1593 cm1 and 1396 cm1 , were corresponding to the vibration
surface area are helpful for the reactant molecules approach to the of C C and C O stretching vibrations, respectively, which
photo-active sites, which could improve the photocatalytic activ- came from the used precursor and solution [39]. While the broad
X. Wang et al. / Applied Surface Science 390 (2016) 190201 195
Fig. 7. Magnetization curve of Fe3 O4 , N-T/CMAC and I0.1 -N-T/CMAC at room temperature.
t 1 t
= + (3)
qt k2 q2e qe
Table 4
Pseudo-rst-order and pseudo-second-order kinetic parameters of SA adsorption onto N-T/CMAC and I0.1 -N-T/CMAC.
Table 5
photocatalytic kinetic parameters of SA solution by different photocatalysts.
Photocatalysts k/min1 R2
3.3.3. Effect of pH, coexisting anion and humic acid (HA) reactive than OH [46]. Hence the presence of Cl and SO4 2 all
It is known that the pH of solution may have inuence on the have negative effect on the photodegradation of SA. Differently, in
adsorption of SA and hence affect the efciency of photocatalysis Fig. 11(c), the photodegradation of SA was strengthened at a lower
[49]. While in groundwater and surface water, there exist vari- concentration of HA (2, 4 and 6 mg/L), and weakened at 8 mg/L. It
ous kinds of negative ions with SA [50,51]. Furthermore, humic is known that HA could serve as a photosensitizer under sunlight
acid (HA) mostly consists of natural organic matter, is also widely or weak irradiation of simulated sunlight [26,50], and HA produces
exist in natural waters, and the concentration of HA is the range reactive species which may enhance the degradation of pollutants
of 0.1200 mg/L [46,49]. In the photodegradation process of pol- [50]. But, excessive HA will inhibited the photolysis process through
lutants, the changing of pH, presence of coexisting anions and HA competitive photoabsorption [55].
may have inuence on the photocatalytic degradation of SA. Hence,
the effects of pH, anions and HA were studied by adjusting pH
of the solutions, adding different concentration of NaCl, Na2 SO4 3.4. Photocatalytic mechanism and reusability of catalyst
and HA for 50 mg/L initial concentration of SA with 2 g/L I0.1 -N-
T/CMAC. From Fig. 11(a), for I0.1 -N-T/CMAC, as the increase of pH To further investigate the underlying photocatalytic mecha-
the removal efciency of SA rst decreases and then increases. At nism, radical and hole trapping experiments were used to detect
pH = 9.0, the extent of degradation becomes the lowest for I0.1 -N- the main oxidative species in the photocatalytic oxidation pro-
T/CMAC. In acidic solution (about pH = 3.0), salicylic acid exists as cess. Tert butyl alcohol (TBA) was used as OH scavengers [56],
molecular form which is favorable for the adsorption, as the solu- and benzoquinone (BQ) was adopted to quench O2 [57]. KI was
tion pH increasing, salicylic acid is ionized to a negative ion and introduced as the scavenger of h+ [56]. From Fig. 12(a), it is clear
then the adsorption capacity of SA decreases rapidly which lower that the addition of scavengers all made the removal efciency
the photodegradation process [52]. In addition, the production of SA decrease. Especially, the presence of TBA and KI made the
of OH radicals could be enhanced under alkaline pH conditions, removal efciency of SA have much more reduce which is 40.6%
which assists in the degradation of SA through OH radical oxida- and 56.69% respectively. As a result, the oxidizing species OH
tion mechanism[53]. In Fig. 11 (b), it is found that Cl and SO4 2 and h+ play more important roles in the degradation process of
all deactivate the photocatalyst as the increase of concentration. SA with I0.1 -N-T/CMAC, and the photodegradation mechanism of
Some researchers reported that Cl anion could act as scavenger of prepared material is shown in Scheme 1. The reusability of I0.1 -N-
positive holes (h+ ) and OH especially in acidic pH [51,54], while T/CMAC was tested with ve times run and the results are shown in
the reaction between sulfate with hydroxyl radical and/or positive Fig. 12(b). After ve times run, the degradation rate of SA still keep-
holes, leading to the formation of ionic radicals SO4 which is less ing high photocatalytic performance (75.78%), which is important
for the application in wastewater treatment.
X. Wang et al. / Applied Surface Science 390 (2016) 190201 199
I0.1 -N-T/CMAC had high specic surface area of 199.3 m2 /g. SEM-
EDS and TEM analysis indicated that TiO2 was well coated on the
surface of magnetic activated carbon. FTIR, XPS, UVvis and PL
studies indicated the decorating of carbon and doping of iodine,
nitrogen happened, hence the prepared material had a better light
absorption in visible light region and the charge separation was
enhanced. Moreover, the prepared material could be easily sepa-
rated by an additional magnetic eld. The photodegradation rate
Fig. 11. Photodegradation of SA with initial concentration 50 mg/L by using I0.1 -N-
T/CMAC with different pH (a), in the presence of chloride, sulfate anions (b) and HA of SA (30 mg/L) on I0.1 -N-T/CMAC composites was 0.0084 min1 ,
(c). which is about 4 times higher than that of N-T/CMAC under visi-
ble light. Increase of SA initial concentration made the degradation
rate of SA decrease. As the increasing of pH, the removal efciency
4. Conclusions of SA rst decreases and then increases. Coexisting anions such as
Cl and SO4 2 have negative inuence on the photo-degradation
Magnetically separable photocatalyst I0.1 -N-T/CMAC was pre- of SA. But suitable concentration of humic acid could enhance the
pared through coprecipitation and sol-gel method. Beneting from photodegradation of SA. In the photodegradation process, OH and
the doping of iodine, I0.1 -N-T/CMAC presented better adsorption h+ are the main oxidative species. I0.1 -N-T/CMAC still own good
and photocatalytic performance. XRD analysis conrmed that the photocatalytic activity after ve times run and it can be used in the
TiO2 supported on activated carbon are mainly anatase phases. degradation of SA from surface water.
200 X. Wang et al. / Applied Surface Science 390 (2016) 190201
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