International Journal of Chemical

& Petrochemical Technology (IJCPT)

ISSN(P): 2277-4807; ISSN(E): 2319-4464
Vol. 4, Issue 6, Dec 2014, 1-12
TJPRC Pvt. Ltd.

REMOVAL OF METHYLENE BLUE FROM AQUEOUS SOLUTION

BYBIVO4/MCM-41 NANOPARTICAL
AWADI. AHMED, A. A. IBRAHIM & F. TH. EL-SHORIFI
Department of Chemistry, Faculty of Science, Mansoura University, Mansoura, Egypt

ABSTRACT
BiVO4/MCM-41nanocatalystsis successfully synthesized viahydrothermal method to enhance the catalytic
activity of MCM-41. The nanocatalysts were characterized by Fourier transform infrared spectroscopy and X-ray
diffraction.

The

adsorption

performance

of

BiVO4

/MCM-41

for

adsorption

of

methylene

blue

is

investigated.BiVO4/MCM-41nanocatalysts reveal enhanced adsorption activity for methylene blue in water as compare to
pure MCM-41 catalyst. Theresults indicate that the adsorption capacity of BiVO4/MCM-4 nanocatalysts for adsorption of
methylene blue increases with the modification of MCM-41 by nanoBiVO4 from 3wt% to 25wt% BiVO4 content, the
sample of 25wt% BiVO4 loaded on MCM-41 shows higher adsorption activity and adsorption capacity.

KEYWORDS: Adsorption, Methylene Blue, Nanopartical, Bivo4, MCM-41

INTRODUCTION
It is well known that heterogeneous catalysts, an ideal green chemistry, have been widely investigated for its
using in environmental applications
and plastics, etc

[2]

[1]

. Dyes are widely used in industries such as textiles, leathe, printing, food,

.Conventional methods for the removal of dyes from wastewater include adsorption onto solid

substrates, chemical coagulation, oxidation, filtration and biologiacal treatment. Adsorption is one of the effective
separation techniques to remove dilute pollutants as well as offering the potential for regeneration, recovery and recycling
of the adsorbing materials

[3-5]

. Methyleneblue (MB), a cationic dye, has wide applications, which include paper coloring,

cotton or wool dyeing, and coating for paper stock, Methylene blue dye has been selected in the adsorption researches,
owing to its widespread, adsorbed by most surfaces in the form of ionic micelles and represents amedium sized adsorbed
molecule of pore size>13Ao.Methyleneblue have been recommended as one of the selected dyes due to many
advantage[6,7]. The removal of dyes from wastewater is an extremely complex problem due to the wide range of
dyeschemical structure and properties and due to essentially nonbiodegradation nature of most dyes[8].
The mesoporousmaterials with surface area are good catalysts and large potential application in the chemical industry and
adsorption processes for remove environmetal pollutants from water, petroleum refinery industry and in heterogeneous
catalysis

[2-4,9,10]

, Especially MCM-41 has been believed the promising materials as adsorbents for various inorganic ions

and organic dyes

o

[11-15]

. The MCM-41materials consist of uniform, hexagonal arrays of mesoporuos with pore diameter

between 2-50A , they show extraordinary high surface areas and narrow pore size distribution

[16-23]

.Metal oxide on

MCM-41 has attracted researcher,tremendous interest,for using in organic pollutants adsorption,because of its high
adsorptionactivaty and high adsorption capacity, high surface area and samall particles size. Moreover, it is also considered
as one kind of excellent catalysts [24,25]. It is known that BiVO4 mainly exists in three crystalline phases, tetragonal zircon,
monoclinic scheelite, and tetragonal scheelite structure, these three crystalline types can undergo phase transition under
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Awadi. Ahmed, A. A. Ibrahim & F. Th. El-Shorifi

different thermal condition

[26, 27, 28]

. The yearsdecate BiVO4 was well-known for applications in pigments because that

BiVO4is anon-toxic yellow pigment which has been consideredas a very interesting alternative
studiesusing of BiVO4 catalysts or photocatalysis, such as BiVO4/TiO2

[30]

[31]

,Ag doped BiVO4 film

[29]

. There are a lot of

,BiVO4/Fe3O4[32].

In the present study, nanopartical BiVO4/ MCM-41 composite catalysts were synthesized by hydrothermal
methed, then characterized by FT-IR and XRD. The prepared samples were usedfor removal of methylene blue dyeas
typical organic pollutant.

EXPERIMENTAL
Materials
All organic and inorganic chemicals used in preparation of photocatalystare: tetraethoxysillane (TEOS),
cetyltrimethylammonium bromide (CTAB), ammoniahydroxide solution (33%), bismuth nitrate pentahydrate
(Bi(NO3)3.5H2O), Ammonia metavanadate(NH4VO4), Methylene blue dye, Dionized water was used in all experiments.
Preparation of the Nanocatalysts
Preparation of Mesoporous MCM-41
Pure silica MCM-41 was synthesized according to the original method that proposed by Beck et al.[6]. 2.0 g CTAB
are added to 100 ml of H2O with stirring until a clear solution and then we added 12.5 ml 33 wt% ammonia solution in
water. Addition of ammonia solution results in a sufficiently basic solution with a pH of 13.0 to 14.0. After vigorous
stirring for about 30 minutes, 10.0 ml of TEOS are then added. At higher TEOS loading, a thick white solution is formed
which generally necessitates manual stirring to ensure adequate gel homogeneity. The product was filtered, washed with
distilled water and dried in air at 120oC. The product recovered from this stage is then washed thoroughly with distilled
water to ensure removal of excess CTAB and ammonia. The result is a fluffy, white powder. The sample is then dried
overnight at 120C. The mole composition of the gel mixture was CTAB: TEOS: Ammonia: H2O = 0.22: 1.04: 1.39:
44.4.To produce a useful high surface area mesoporous material, the surfactant template is removed via high temperature
calcination, leaving behind a mesoporous silica framework around hexagonally arrayed pores. The calcination procedure
has been optimized to remove the organic template from the catalyst without being so harsh as to destroy the mesoporous
silica skeleton. Samples for calcination are placed in a ceramic vessel and loaded into a muffle at 550C with rate of 5C
per minute for 6 hour period. The sample removed from the furnace is designated MCM-41 and stored in a desiccator
toprevent water adsorption onto the catalyst surface.
Preparation of BiVO4/MCM-41nanocatalyst
A certain amount Bi (NO3)3.5H2O was dissolved in water. After complete dissolution, the solution was added to
Acertain amount of MCM-41 uncalcined(the MCM-41unclcined added to water with stirred for 15 and ultrasonic for
5min),then the mixture was stirred for 30 min at room temperature,afterward acertain amount of NH4VO3 was added to
above mixture and stirred to 2hr. Then dried at 800C in rotary, the obtained powder wascalcined at 5500Cfor 6hr.

CHARACTERIZATION
X-Ray Diffraction Analysis
XRD patterns of all samples were recorded at low and high angle using PW 150 (Philips) using Cu K radiation
source and Ni filter. The instrument was operated at 40 kV and 45mA. The scanning was made for 2 angle from 1 to 70,
with a step size of 0.02 and a step time of 2s. In order to avoid the problem of illuminated area at low 2 angle that may
Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Removal of Methylene Blue From Aqueous Solutionbybivo4/Mcm-41 Nanopartical

affect the positions of the diffraction lines. This peak is indexed to a hexagonal unit cell and used in conjunction with
Bragg's law in calculating d100 spacing for the hexagonal pore network as well as the unit cell parameter (ao). Where the
average crystallite size of particles was determined by XRD line broadening technique using Debye-scherrer
equation:
Where D is crystal size, is radiation wavelength (A0), is the line breadth (radians) and = angle of reflection.
Fourier Transform Infrared Spectra
The FT-IR spectra of MCM-41 modified by nanoBiVO4 were recorded with Nicolit ManagaIR 550 spectrometer
with a 4 cm-1 resolution and 128 scans in the mid-IR region 400-4000cm-1.The sample was mixed and grind with KBr and
compressed into a thin wafer that was placed inside the IR cell and then the infrared specrum was recorded.

RESULTS AND DISCUSSIONS

X-Ray Diffraction Pattern (XRD)
XRD was employed to characterize the crystal phases of nanoBiVO4and BiVO4/MCM-41nanocomposites.
The XRD is similar to those reported in literature indicating that the mesoporous molecular sieves prepared have an
ordered hexagonal structure, Figure 1, represent low angle powder XRD patterns of BiVO4/MCM-41 samples contain
3%,25% and 35% BiVO4. The X-ray diffraction BiVO4/MCM-41 at low angle demonstrate the typical Bragg reflection of
the mesoporous MCM-41 material with hexagonal array, which is evidenced by the diffraction peaks at 2.3,4.0,and4.8
assignable to the (100),(110) and (200) silica planes,repectively[8].However compared with pureMCM-41,the peaks
100,110 of BiVO4/MCM-41 samples widen and weaken obviously, which suggest that the hexagonalorder decreases with
introducing nanoBiVO4 into the framework of MCM-41.This phenomenon indicate that mesoporousof the MCM-41 is
unchanged aftermodification.Inother words, the pore structure of MCM-41was not destroyed during thesolid dispersion
processes[9]. The main different between pure MCM-41 and BiVO4/MCM-41 with different BiVO4 content is the intensity
of BiVO4/MCM-41 diffraction peaks weredecreased slightlywith increasing the BiVO4 content due to pore filling of the
host materal, which reduces the scattering contrast between pore walls and pores, thus leading to a decrease in peak
intensity, the higher the electron density of the sorbate molecule

[9,10]

. The XRDpatterns of high angle are shown in

Figure 2. The peaks appear at 2= 18.8, 28.78, 30.5, 35.2, 39.8, 42.4, 45, 47.2, 50.28, and 53.220, were confirmed
monoclinic scheeliteBiVO4phase according to the standard XRD pattern of monoclinic scheeliteBiVO4phase
(International Center for Diffraction Data,JCPDS No.14-0688). The samples showedsharp and norrowpeaks indicate high
degree of crystallinty in pure BiVO4 nanocomposites

[33-35]

. The results indicate thattheintensity of peak at 2 =28.78

increased with amount BiVO4content.The nanosizes of catalyst nanocomposites are calculated by the Scherrer formula
[36,37]

. The average sizes are about3.6nm, and 3.07 nm for 25wt% and 35wt%BiVO4/MCM-41, respectively, while the

samples pure MCM-41 and 3wt% BiVO4/MCM-41 were amorphous.

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Awadi. Ahmed, A. A. Ibrahim & F. Th. El-Shorifi

Figure 1: Low Angle X-Ray Diffraction Pattern of (a) Pure MCM-41, (b) 3%,
(c) 25% and (d) 35% Bivo4/MCM-41nanocoposites

Figure 2: High Angle X-Ray Diffraction Pattern of (a) Pure MCM-41, (b) 3%,
(c) 25% and (d) 35% Bivo4/MCM-41nanocomposites
FT-IR
Figure 3, shows the spectra of pure MCM-41 as well as 3%, 8%, 15%, 25% and 35% BiVO4/MCM-41 samples
calcinated at 550oCin the region of 4000-400cm-1. Absorptions at 1635cm-1and 3463 cm-1can be ascribed tobending and
stretching vibrations of the adsorbed H2O molecules,respectively[12,13].The strong vibration band at 1069 cm-1 in pure
MCM-41 assigned to asymmetric stretching of Si-O-Si shifted to 1089 cm-1 in BiVO4/MCM-41 samples. Wave number for
asymmetric stretching of Si-O-Si has beenshifted to higher value when BiVO4 was loaded into MCM-41.The Si-O-Si from
MCM-41are observed at1080cm-1to 1250cm-1,960cm-1, 805 cm-1,and 446cm-1, where that the band at 805cm-1and 1095
cm-1obsorved in all samples BiVO4/MCM-41were attributed to symmetric and asymmetric strecheting vibration of Si-O
band, respectively. While a band at 464cm-1indicates the bending vibration of Si-O-Si,and band at 960cm-1 is due to the
Si-Ostrechetingvibration polarized or free vibration of Si-OH band[12,13,4,36].Additionally,the bands at 736 cm-1 and 805
cm-1obsorved at low frequencyare attributed to

(VO4)and

(VO4 )[37,38].

The band960 cm-1 in BiVO4/ MCM-41 sample is more intense as compared to the peak present in pure
MCM-41.the peaks at 805cm-1 in BiVO4/MCM-41 sample is more broad and intense.The peak at 960 cm-1 in pure
MCM-41 is more intense and can be attributed to the silanol Si-OH vibration. The peak 960cm-1 in MCM-41 is also narrow
and more intense due to free vibration of Si-OH bond as compared to BiVO4/MCM-41sample. This indicates that,
nano BiVO4 is bonded tosilca by Si-O-Bi bond.
Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Removal of Methylene Blue From Aqueous Solutionbybivo4/Mcm-41 Nanopartical

Figure 3: FT-IR Spectra of (a) Pure MCM-41 (b) 3%, (c) 8%, (d) 15%,
(e) 25% and (f) 35% Bivo4 /MCM-41 nanocomposite

Removal of Methylene Blue (MB)

Effect of Bivo4 Content
The adsorption of methylene blue (MB) dyewas followed at different time by using 0.1 g of nanocatalyst, and 100
ml of 100mg /L dye solution. Figure 4, shows the effect of contact time from 0-240minson the adsorption efficientcy of
MB dye forall samples, pure MCM-41, 3,8,15,25,and 35%BiVO4/MCM-41 nanocomposite.The removal of MB dye
increaseswith thecontact time andgradually reach to equilibrium after 60 mins.The removalofMB dye by thesamples of
nanocatalystswere quick increases during the first 30 mins,then gradual increases during 60 mins.The maximum removal
effecints of dye were 49.38, 92.1, 94.79%, 96.3%, 99.85, and 93.98 % for MB dyeon pure MCM-41, 3%, 8%, 15%,
25%,and 35% BiVO4/MCM-41nanocatalysts,respectively.The results indicated that BiVO4content playsa signification role
on the catalytic activity of MCM-41catalysts. The % removal of dye increases with BiVO4content until 25%. This is may
be attributed to the electrostatic interaction between BiVO4/MCM-41 with negative charge and MB with positive charge.
The lower removal of methylene blue at35% BiVO4/MCM-41, due to the abundance of OH group competing with MB
molecules for the adsorption sites.

Figure 4(a): Effect of Bivo4 Content on Adsorption of MB after 240 Min

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Awadi. Ahmed, A. A. Ibrahim & F. Th. El-Shorifi

Figure 4(b): Effect of Bivo4 Content on Adsorption of Mbafer 60 Min

Effect of Initial Dye Concentration
The effect of initial concentrations of MB dye,on the removal rate at initial dye concentration 25,50,100,200 and
300 mg/L in 4hr by using 0.1g BiVO4/MCM-41nanocatalystare shawn in Figure 5. It is well document that the intial
concentration of the MBsolution is dominant factor in determining the adsorption capacity of the adsorption. In the present
investagetion , the adsorption of MB at 25oC from non buffered solutions of 25,50,100,200 and 300 mg/L keeping the
adsorptent 25% BiVO4/MCM-41 dosage constant.Evidently, with the solution of Co=25,50,100,200 and 300mg/L,
the maximum uptake was100%,100%,99.23%,79.55%,and 67.585 %,respectively.This may be attributed the fact that the
increase of the initial concentration of adsorbate represents a driving fore for adsorption. However, one may take into
concideration that inspite of the increase of adsorption capacity of 25% BiVO4/MCM-41 sorbent, the precrntage removal
was found to decrease with the increase of intial concentrationof MB from 25,50,100,200 to 300 mg/L.For the lower MB
solutions concentrations, the % removal amount to about 100%, i.e. approaching complete removal of the dye.The decrease
of the % removal of dye at C0=300 mg /Lmay be attributed to the saturation of the available active site with the increase of
intial concentration of MB.

Figure 5: Effectof Initial Dye Concentration on Adsorption of MB

Effect Ph on Adsorption of MB
Figure 6, depicts % remoavl versus pH for 25wt% BiVO4/MCM-41 calcined at 5500C.Evidently, successive
increase of adsorption of MB is shown with the increase of pH from 2 to 10.Adsorption of MB dye by nanocatalysts is
Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Removal of Methylene Blue From Aqueous Solutionbybivo4/Mcm-41 Nanopartical

affected by the characteristic of the BiVO4/MCM-41 surface and structure of dye molecular. Considering now the effect of
dye solution pH, one can assume lower adsorption of MB at acidic pH is probably due to the presence of excess H+ ions
competing with the cation groups on the dye for adsorption sites.The adsorption can also be explained on the basis of an
electrostatic interaction between the ionic dye molecule and charged substrate.

Figure 6: Effect of Ph Dye Solutionon the Adsorption Properties

Effect of Catalyst Weight
The adsorption of MB dye by BiVO4/MCM-41 nanocatalysts were studied by changing amount of the catalyst
weight 0.05g, 0.1g , and 0.2g with keeping initial dye concentration 100 mg/L for 240mins.The effect of catalyst weight on
adsorption of MB dye is shown in Figure 7. The results rveal that the adsorptionprecent removal of MB increased from
85.8, to, 99.85, then to 100% with increasing the catalyst weight from 0.05g, to, 0.1g, then to, 0.2 grespectively.
The maximum adsorption efficiency was 100% for MB with 0.02g of catalyst.This indicates that, as amout of catalyst
weight increases, the ability of the catalyst to adsorption of MB increases.

Figure 7: Effect of Catalyst Weight on Adsorption of MB

Effect of Tempeture on Adsorption of MB
The effect of temperature of the removal of MB was studied, at temperatures 250C, 350Cand 450C in 240mins by
using 0.1g BiVO4 / MCM-41nanocatalyst. Figure 8, showsthe effect of temperatureon the adsorption of MB dye.
The results rveal that the adsorptionprecent removal decreases from 99.85, to,85.31, then to,76.98 with increasing in the
temperature from 250C, to 350C, then to, 450C respectively.The maximum adsorption efficiency was 99.85% for MB with
250C,indicates that adsorption of MB on BiVO4/MCM-41 was physical adsorption.
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Awadi. Ahmed, A. A. Ibrahim & F. Th. El-Shorifi

Figure 8: Effect of Temperature on the Removal of MB by Nano BiVO4 Loaded on MCM-41

Effect of Calcination Temperature of Nanocatalystson the Removal
Figure 9, shows the % removal of MB by BiVO4loaded on MCM-41 nanocatalyt, at 4500C, 5500C, 6500C for the
sample 25%wt BiVO4/MCM-41nanocatalysts.The resultsindicate that the calcination temperature5500C was the best
temperature forthe performance catalysis, and results, also clarified that the sample 25% BiVO4/MCM-41 nanocatalysts
has the highest adsorption activity.

Figure 9: Effect of Calcination Temperature of Nano BiVO4 Loaded

on MCM-41 Uncalcined on Adsorption of MB

CONCLUSIONS
BiVO4/MCM-41nancatalyst with different nanoBiVO4 content were synthesized by hydrothermal method. XRD
results revealed that the BiVO4 crystals were of monoclinic scheelite type loaded on MCM-4, change the hexagonal
sturcture of mesoporous silica. FT-IR results confirmed the presence of BiVO4 in BiVO4/MCM-41 nanocatalysts.
All pnanocatalysts prepared exhibited catalytic activity, BiVO4content of 25 % was the optimum condition for the
preparation of best performing BiVO4/MCM-41nanocatysts characterization by the adsorption of MB. The percentage
remopval of MB increased with with BiVO4 content till an optimum BiVO4content of 25% BiVO4 loaded on MCM-41.
All expermetal and characterization were conformed that Thesamples of 25% nanocatalyst showed an enhanced
crystallinity with the crystallite size ranging from 3.6, and enhanced catalytic activety and adsorption capacity reached to
94.3 % and99.85 % for MB adsorption on nanocatalyst after 60min and 240 mins, respectively.

Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Removal of Methylene Blue From Aqueous Solutionbybivo4/Mcm-41 Nanopartical

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Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

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