Open Journal of Polymer Chemistry, 2012, 2, 6-13

http://dx.doi.org/10.4236/ojpchem.2012.21002 Published Online February 2012 (http://www.SciRP.org/journal/ojpchem)

Selectivity of Acrylic Acid Radiation Grafted Non-Woven

Polypropylene Sheets towards Some Heavy Metals Ions
Dalia El-Sayed Hegazy
National Centre for Radiation Research and Technology, Cairo, Egypt
Email: Dalia_eahegazy@ Yahoo.com

Received December 27, 2011; revised January 27, 2012; accepted February 5, 2012

ABSTRACT
Graft polymerization has been considered as a general method for the modification of the physical and chemical proper-
ties of polymeric materials and of particular interest for synthesis of the hydrophilic membrane. In this study, hydro-
philic carboxylic acid groups were introduced by radiation-induced grafting of acrylic acid (AAc) onto non-woven
polypropylene fabric (NWPP). Different irradiation doses and (AAc) monomer concentrations were used to optimize
grafting yield. Characterization and properties of the prepared graft copolymer were studied by employing X-ray Dif-
fraction (XRD), Thermogravimetric Analysis (TGA), Scanning Electron Microscope (SEM ), Fourier Transform Infra-
red Spectrometry (FTIR) and differential scanning calorimeter (DSC). The prepared grafted materials were used for
removing some heavy metals ions. The results showed that the non-woven PP grafted with (AAc) has good affinity to-
ward Cu, Ni and Co.

Keywords: Radiation Grafting; Acrylic Acid; Characterization; Removal of Heavy Metals

1. Introduction base polymer matrix. Moreover, the molecular weight of

the products can be better regulated in radiation tech-
Water contamination with toxic metals causes serious hu-
niques In general; synthesized polymers such as polyeth-
man health problems. Enhanced metal separation tech-
ylene and polypropylene have been used as trunk poly-
niques that require less energy with minimal impact on
mer due to their reactivity in the grafting process and
the environment are desirable. Many kinds of metal ads-
high mechanical strength.
orbents including activated carbon, bentonite and synt-
Non-woven materials have been increasingly used for
hetic polymers have been developed to remove toxic me-
a variety of applications in the world [5]. Non-woven
tals from streaming water [1]. Radiation-induced graft
materials are one of the products popularly used as rein-
polymerization is widely used to produce high perform-
forcements for many applications since they possess a
ance chemically active polymer materials for adsorption
and separation processes on the basis of various com- good combination of strength, lightweight and flexibility
mercial polymers available in different forms (films, fi- compared to conventional materials [6]. Non-woven with
bers, resins, textiles, powders) [2,3].Various approaches specific surface properties are also of interest in many
for synthesizing polymer adsorbents have been devel- technical applications of the materials as the surface fea-
oped, including direct graft polymerization of vinyl mo- tures affect adsorption, abrasion, adhesion, biocompati-
nomers already containing desirable functional groups. bility and other properties of the materials. The advan-
Adsorbents can be easily synthesized by radiation-induced tages of using nonwoven polypropylene NWPP as matrix
graft polymerization. This technique creates an active are their relatively low processing temperature which is
radical in the trunk polymer by means of ionizing radia- essential because of low thermal stability of natural fi-
tion and the polymeric graft chains propagate from the bers and their good properties and lower cost. For these
active radical in the trunk polymer [3,4]. Chemical initia- increasing applications it is desirable to produce such
tion often brings about problems arising from local heat- nonwoven materials with well defined surface properties.
ing of the initiator, an effect that is absent in the forma- Various techniques have been developed to modify the
tion of free-radical sites by radiation, which is only de- surface properties of nonwoven materials [7-9].
pendent upon the absorption of high-energy radiation. In recent years, the removal of hazardous heavy metals
Due to large penetrating power of higher energy radia- from water and soil environments and industrial waste
tion, methods using radiation initiation provide the op- streams has attracted considerable attention. Enhanced
portunity to carry out grafting at different depths of the metal separation techniques that require less energy with

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 D. E.-S. HEGAZY 7

minimal impact on the environment are desirable. amount of transition metal ions are commonly used as
In the present work, radiation grafting of AAc mono- inhibitors (1), ammonium ferrous sulfate (Mohr’s salt)
mer onto non-woven polypropylene fabrics is investi- was added to the reaction medium (0.5 wt%).
gated to obtain homogeneous distributed graft copolymer
chains with high grafting yield. Characterization and pro- 2.4. Fourier-Transform Infrared (FTIR)
perties of the prepared graft copolymer are studied by
To justify the introduction of functional groups onto the
(XRD), (TGA) and (DSC). Also, the study included
nonwoven PP, infrared spectroscopy analysis was carried
measurements of the mechanical properties and determi-
out using a FTIR spectrometer. The infrared spectra of
nation of the tensile strength of these materials as a func-
NWPP and grafted NWPP sheets were performed using
tion of degree of grafting. The application of the pre-
Jasco 6300FT-IR.
pared NWPP-AAc as adsorbent materials for waste water
treatment from heavy and toxic metals is investigated.
2.5. Thermogravimetric Analysis (TGA)
2. Experimental TGA for the investigated samples were performed under
nitrogen atmosphere at a flow rate 50 ml/min. of pure
2.1. Materials
nitrogen gas and the heating rate was 10˚C/min. from
The materials used in this study were needle punched ambient temperature up to 600˚C using Perkin Elmer
nonwovens made of melt blown nonwovens extruded system of type pyris-6 thermal analysis system.
from PP polymers. Film sheets were cut to the dimention
of 4 × 5 cm. The monomer used throughout this work 2.6. DSC Measurements
was acrylic acid (AAc) of laboratory grade chemicals of
Thermal parameters of the prepared grafted NWPP such
purity 99% (Merck).
as; melting temperature (Tm) heat of melting and recrys-
tallization (ΔHm) were determined by differential scan-
2.2. γ-Irradiation
ning calorimeter (DSC) (Perkin Elmer equipped with a
Irradiation to the required doses was carried out using a DSC-7 data station). Specimen (≈5 mg) of the sample is
60
Co γ-cell. The irradiation facility was constructed by used for DSC measurements. Indium and Zinc standards
the National Center for Radiation Research and Tech- were utilized to calibrate the temperature and thermal
nology, Atomic Energy Authority of Egypt. Irradiation scale. The measurements were carried out in N2 atmos-
was carried out in air atmosphere at different irradiation phere at a heating rate of 10˚C min–1.
doses.
2.7. X-ray Diffraction Analysis (XRD)
2.3. Radiation Grafting of Non-Woven
X-ray diffraction (XRD) patterns were recorded using
Polypropylene
Shimadzu X-ray diffractometer (XRD-6000 model) equip-
NWPP sheets were washed with acetone, dried at 50˚C in ped with X-ray tube at operating voltage of 40 kV and an
an electric oven until they attain a constant weight and electric current of 30 mA.
then immersed in the monomer solution in glass tubes.
Distilled water was used as a diluent of AAc. The graft 2.8. Mechanical Properties
copolymers were prepared by direct radiation grafting of
AAc onto NWPP at different irradiation doses. The Tensile tests were performed according to the ASTM
grafted films were removed and washed thoroughly with D412-80 test method and were carried out using an In-
the proper solvent (hot distilled water) in order to extract stron testing machine (Model H10KS from Hounsfield
the residual monomer and homopolymer which may be Co., England, loaded cell 10 KN) at 25˚C and the cross-
accumulated in the film and then soaked overnight in head speed was 10 mm/min. Five samples per formula-
distilled water. These prepared grafted polymers were tion were tested.
then dried in an electric oven at 40˚C for 24 h and
weighed. The degree of grafting was calculated using the 2.9. Metal Uptake Measurement
following equation: The fixed weight of the prepared hydrogel was immersed
Wg  W0 in the metal feed solution of definite concentration (100
Degree of grafting  %   100 (1) ppm). Merck atomic absorption standard solutions of
W0
these metals were used for the calibration process. The
where W0 and Wg represent the weights of initial and pH and temperature of metal feed solutions were ad-
grafted film, respectively. justed before applying the hydrogels for treatment proc-
To overcome homopolymerization of AAc, a small esses. The remaining metal ions in its feed solution were

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8 D. E.-S. HEGAZY

determined by an atomic absorption instrument (Unicam 65

Model Solaar 929). 60

The metal uptake (E) was calculated as follows:
Ci  C f

Degree of grafting (%)

55
E (mmol/g)  (2)
W  A 10 50

where W is the weight of the dried grafted film, A is the

45
atomic weight of metal ion and Ci and Cf are the initial
and remaining concentrations of metal ions in mg/l (ppm), 40
respectively. The total uncertainly for all experiments
ranged from 3% - 5%. 35

3. Results and Discussion 0 10 20 30 40 50 60 70

AAc concentration (wt%)

The radiation grafting process of aqueous AAc is usually
Figure 1. Effect of aqueous AAc concentration on the de-
accompanied by undesirable homopolymerization. Metal
gree of grafting onto NWPP at irradiation dose (30 kGy).
salts such as ammonium ferrous sulphate (Mohr’s salt),
suppress homopolymer formation. Fe2+ is well known to 120
have an inhibition effect on free radical graft polymeriza-
tion. However, they can also cause a deactivation of the 100
grafting process and lead to a decrease in grafting degree
Degree of grafting (%)

when taken in excess. In the present study, it was found 80

that the addition of 0.5 wt% of Moher’s salt to the aque-
ous AAc is enough to enhance radiation grafting and 60

minimize the homopolymer formation.

40

3.1. Effect of Monomer Concentration on the

Grafting Yield 20

Among the effective parameters for radiation grafting are 0

the monomer concentration. The effect of AAc monomer 0 10 20 30 40 50

concentration on the grafting yield was investigated as Irradiation dose (kGy)

shown in Figure 1. It is clear that the degree of grafting
Figure 2. Effect of irradiation dose on the degree of grafting
increases by increasing AAc acid to reach a maximum at of AAc (30 wt%).
30 wt% AAc. Thereafter, any increase in monomer con-
centration leads to decrease in the grafting degree. At 30 irradiation dose leads to more free radical formation in
wt% AAc, there is enough monomer available to reach the grafting sites which leads to an increase in the gra-
into the reaction sites on the polymer free radicals, re- fting yield. However, at irradiation doses above 30 kGy,
sulting in higher degrees of grafting. The excess of mo- the content of crosslinked insoluble homopolymer in-
nomer concentration causes suppression of the monomer creased and it was difficult to extract it from the surface
diffusion by increasing the viscosity of the grafting me- of NWPP sheets [11]. Also, a degraded rigid grafted
dium under the homopolymerization effect (the Troms- NWPP sheets was formed at high irradiation dose.
dorff effect) [10].
3.3. Swelling Behavior of the Grafted NWPP in
3.2. Effect of Irradiation Dose Water
Irradiation dose is also an important factor to optimize From the practical point of view, the swelling properties
the grafting process and homogeneity of grafting distri- and its ratio is very important property for its use in
bution. This is due to the initiation of grafting sites and treatment process of waste water and diffusivity of met-
growing chain reactions are very dependent on the amount als through the grafted chains and functional groups. The
of free radicals formed. The effect of irradiation dose on swelling of the prepared NWPP-g-AAc copolymer in
the grafting yield of AAc onto NWPP was investigated water was studied and the results are presented in Figure
and is shown in Figure 2. It is obvious that as the irra- 3. It can be shown that as the degree of grafting increases,
diation dose increases, the grafting degree increases. This the swelling percent increases to reach a maximum at
trend can be explained to the fact that the increase in the degree of grafting around 100%. Thereafter, the swelling

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 D. E.-S. HEGAZY 9

450

400

350
Swelling (%)

300

250

200

150

100

50
40 60 80 100 120 140

Degree of grafting (%)

Figure 3. Swelling percent vs. degree of grafting percent for
NWPP-g-AAc at swelling time (24 h).

percent tends to decrease with further increase in the gr- Figure 4. FTIR spectra for (a) NWPP; (b) NWPP-g-AAc.
afting yield. As the irradiation dose increases, the increase The AAc concentration (30 wt%) and degree of grafting
(64%).
in degree of grafting and cross-linking density which pre-
vents a space for the AAc chain to swell freely in water
and restricts and hindered the diffusivity of water thro-
ugh the cross-linked chains is expected. In other words,
results showed clearly that the increase of irradiation dose
during radiation grafting process enhanced the crosslink-
ing via hydrogen bonding. As a consequence, the water
uptake tends to decrease at high degrees of grafting.

3.4. FTIR Analysis

The FTIR spectra of the original NWPP and grafted
NWPP films were studied and shown in Figure 4. FTIR
spectrum of pure NWPP shows bands appearing at 2840-
2800, 1440 and 1380 cm–1, which are characteristic of the
polypropylene structure. In case of NWPP-g-AAc, a new
Scheme 1. The expected structure of NWPP-g-AAc
peak appears at around 1715.67 cm–1, which can be at-
tributed to the –C = O of PAAc. A characteristic peak 100
around 3500 cm–1 for OH groups of poly acrylic acid is
also appeared. This confirms that acrylic acid containing
90
the carboxyl groups was fixed randomly onto the NWPP
main chains as a grafting side chains [12-14]. Scheme 1
Elongation (%)

shows the expected structure of NWPP-g-AAc. 80

3.5. Mechanical Properties

70

Figures 5 and 6 show changes in percentage elongation

and tensile strength at break for grafted and ungrafted
60
NWPP films, respectively. It can be seen that the elonga-
tion percent at break for the grafted non-woven sheets de-
creases gradually as the grafting degree increases. How- 50

ever, the tensile strength increases with increasing the 40 60 80 100 120 140

degree of grafting up to 66% grafting degree, thereafter, Degree of grafting (%)

any increase in the grafting degree leads to de crease in ten- Figure 5. Elongation percent at break for NWPP-g-AAc
sile strength. The decrease in the percentage elongation having different degrees of grafting.

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10 D. E.-S. HEGAZY

Table 1. DSC results of NWPP-g-AAc.

Grafting degree (%) Tm ΔHm

0 160 61.9

66 157 14.5

93 155.8 16.6

130 153.8 5.7

shown in Figure 7 and Table 2. The results show that

the thermal stability of NWPP films has been changed by
grafting with AAc. The grafted films exhibited two de-
composition peaks, i.e., the first decomposition occurring
Figure 6. Tensile strength at different degrees of grafting. at around 200˚C - 235˚C may be due to cyclization and
dehydration reactions of -COOH functional groups of the
and the improvement in the tensile strength is expected grafted chains. The decomposition of the second peak
due to the increase of crosslinking sites with increasing should be attributed to the decomposition of the grafted
the number of grafted chains and their lengths [15,16]. film and due to extensive graft chains degradation of the
The cross-linked network structure resulted in a pro- polymer backbone chain.
nounced increase in the tensile strength of grafted sheet It is evident from the thermograms that the ungrafted
in the range from 60%-100% grafting and as consequ- NWPP is thermally stable up to 236˚C.The grafting of
ence the percentage elongation decreased [17,18]. Again, AAc onto NWPP decreases the weight loss of the major
the rigidity of the graft copolymer increases with an in- degradation step compared to that of the ungrafted
crease in degree of grafting due to two reasons; the first NWPP as shown in Table 2. A considerable decrease in
one is the incorporation of the polar groups and their the weight loss of the major degradation step is observed
interactions (the formation of cross-linked network struc- systematically by increasing degree of grafting. The ana-
ture via hydrogen bonding of carboxylic acid groups of lysis of the thermograms shows that the degradation of
PAAc graft chains). The second reason is the formation grafted polymer is controlled mainly by the degree of
of crosslinking network structure, which formed because grafting. In conclusion the introduction of AAc into
of grafting and irradiation, which leads to restriction in NWPP sheets does not affect significantly the thermal
chain mobility [18-20]. The decrease in the tensile stability of the NWPP sheets.
strength of high grafted yield non-woven sheet prepared
at high irradiation dose was due to the degradation of 3.8. X-ray Diffraction Analysis (XRD)
polypropylene non-woven sheet caused at high irradia-
X-ray diffraction of the grafted NWPP was performed
tion dose.
and compared with the base polymer to clarify their
crystallinity morphological structures changes caused by
3.6. DSC Thermal Parameters of Grafted NWPP
the grafting as shown in Figure 8. It is observed that the
In order to determine the effect of grafting degree on the intensity of the diffractogram, representing crystallinity,
thermal parameters of the grafted NWPP, the change in decreases by grafting. This is due to dilution of the crys-
Tm and ΔHm was investigated by DSC technique and is tal line fraction by the incorporation of the amorphous
shown in Table 1. The decrease in Tm and ΔHm values PAAc chains into the polymer matrix. It can be con-
for the grafted NWPP films compared with ungrafted cluded that the graft polymerization took place predomi-
ones can be attributed to the network structure, which nantly on the polymer film surface of the crystallites pro-
had considerable mobility with the molten NWPP. The gressed inward thus breaking up partly ordered chain
results obtained, suggested that the introduction of gra- structures of the NWPP matrix [21].
fted chains into NWPP caused changes in its morpho-
logical structure in which the crystallinity domains in 3.9. Selectivity of NWPP-G-Aac towards
NWPP decreases due to the crosslinking network forma- Different Metals in Mixture
tion that caused by radiation grafting process.
Because of functional groups, which have been introduced
into polymer to be used as chelating polymer, the capacity
3.7. Thermogravimetric Analysis (TGA)
of the polymer is an important factor to determine how
The thermograms for the NWPP and grafted NWPP are much such graft copolymer is required to quantitatively

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 D. E.-S. HEGAZY 11

metals and follows the order Cu > Co > Ni as shown in

Figure 9(a). The results show that the NWPP-g-AAc has
a great ability to adsorb Cu rather than other metals un-
der investigation.

250

200

Capacity(mg/l/gm)

Cu
150

Co
100

Ni
50

Figure 7. Thermogravimetric curves of pure NWPP and the

0
grafted NWPP sheets.
Ni Co Cu
Table 2. TGA data for PP-g-AAc. (a)
250
Grafting Onset Char residue Wt. loss in the major
degree (%) temperature (˚C) (%) degradation step (%)
0 236 2.5 90.5 200
57 225 2.3 89.8
Capacity(mg/l/gm)

Co
66 220 2.1 87
150
93 215 1.5 87
Cu

Co
100

Ni

Ni
Cu
50
50 kGy
Intensity (arbitrary unit)

30 kGy Cu/ Co Cu/ Ni Co/Ni

(b)
20 kGy 160

140
Co

10 kGy
Capacity(mg/l/gm)

120

100
Ni

0 kGy 80
Cu

60

10 20 30 40 50 60 70 80 90 40

2 (deg) 20

Figure 8. XRD patterns for NWPP-AAc graft copolymers 0

prepared by gamma irradiation at different doses. Cu-Co-Ni

(c)
remove a specific metal ion from the solution. Thus, the
Figure 9. (a) The capacity of NWPP-g-AAc towards differ-
capacity of NWPP-g-AAc towards different metals such ent metals; (b) The selectivity of Cu in presence of Ni and
as Cu, Co and Ni was determined and is shown in Figure Co ions; (c) The selectivity of the prepared NWPP-g-AAc in
9. The NWPP-g-AAc has a good affinity towards such a mixture Co, Cu and Ni.

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12 D. E.-S. HEGAZY

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