International Journal of Eco-Innovation in Science and Engineering Vol 3 .
, 2022 .
https://ijeise.
id/ E-ISSN: 2721-8775 Article Poly (N-tert-amylacrylamide -co- Acrylamide/ Sodium acrylat.
Fe3O4 Nanocomposite Hydrogels as polymer catalyst for the reduction of Methylene Blue Dye Pazhnaisamy1* .
Euis Nurul Hidayah2 and Indra Sulania3 1Department of Chemistry.
Sir Theagaraya College (Affiliated to University of Madra.
Chennai-600021.
India.
2Department of Environmental Engineering.
University of Pembangunan National AuVeteranAy Jawa Timur.
Surabaya.
Indonesia.
3 Material Science.
Inter-University Acceleration Centre.
New Delhi-110067.
India *Corresponding author: .
_pazhanisamy@yahoo.
|Phone number: - Received: 17th November 2022.
Revised: 21st November 2022.
Accepted: : 23rd November 2022.
Available online: November 2022.
Published regularly: May and November.
Abstract Fe3O4 Nanocomposite Hydrogels were prepared by free radical polymerization using N-tert-amyl acrylamide .
Acrylamide and Sodium acrylate monomers at 60OC.
Fe3O4 NPs was intercalated via in situ The synthesized nanocomposite Hydrogels conformed by FT-IR spectroscopy.
Surface morphology of the nanocomposite hydrogels indicated the ferrate nanoparticles are intercalated uniformly throughout the polymer matrix.
The XRD pattern of the hydrogel showed the presence of nanoparticles in the matrix with certain crystallinity nature.
UV-visible absorption studies reveal the catalytic activity of Methylene Blue dye molecules in the aqueous medium by the Nanocomposite Keywords:
Introduction Hydrogels are three dimensional polymeric network in which there are a lot of hydrophilic groups, those swell quickly by imbibing a large amount of water or de-swell in response to changes in their external environment .
They have found wide application in bio-medical materials as well as drug control and release.
Hydrogels can swell to profitable rates when placed into an appropriate environment, which means a specific pH ,temperature, electric field,light,pressure or specific molecule .
Hydrogels exhibiting pH sensitive swelling behavior have been usually swollen from ionic network that contain acidic or basic pendant When these groups are ionized, a swelling osmotic pressure inside the material is built up and fixed charges are trapped in the gel.
As a result of the electrostatic repulsion ,the uptake of solvent in the network is increased.
Fe3O4 known as magnetite is one of the oxides of iron which plays a major role in various areas of chemistry, material sciences, physics and medical sciences.
Fe3O4 crystallizes in mixed oxidation state iron (Fe3 and Fe2 ) inverse cubic spinel structure .
Fe3O4 can be used in magnetic resonance imaging, in drug delivery systems, as sorbent for heavy metal, as antibacterial agents, as catalyst, as electrochemical biosensors, as shielding material in electromagnetic interference and for energy harvesting .
It has been reported that separation between valence band of Fe.
and O.
in Fe3O4 is 4Ae6 eV .
-206 n.
The aim of this work is to prepare a series of poly(Ntert-amylacrylamide-co-acrylamide/AcN.
Fe3O4 Hydrogels, based on NTA ,acrylamide and sodium acrylate and to study the swelling behavior of Hydrogels.
Hydrogels were prepared by freeradical crosslinking polymerization of NTA,AM DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering Vol 3 .
, 2022 and AcNa in the presence of N,NAo-methylenebis acrylamide(MBA) as the cross linker Material and Method 1 Materials Acrylamide (AM.
Merc.
was crystallized from acetone/ethanol mixture.
Acrylic acid was distilled twice by vacuum distillstion at 63 0C/25 mmHg and stored in a refrigerator.
Sodium acrylate was prepared by neutralizing the acrylic acid using sodium hydroxide.
The crosslinker N,N'-methylene-bis-acrylamide (MBA) was used as received.
Acrylonitrile was first washed with 5% NaOH solution in water to remove the inhibitor and then with 3% Ortho phosphoric acid solution in water to remove basic impurities.
Then the Acrylonitrile was washed with double distilled water and dried over anhydrous CaCl2.
The acrylonitrile was then distilled in an atmosphere of Nitrogen and reduced pressure.
It was then collected in a clean dry amber colored bottle and kept in the refrigerator at 5C 2 Preparation of N-tert-amylacrylamide (NTA) The monomer N-tert-amylacrylamide(NTA) was prepared by the reaction of t-amyl alcohol with acrylonitrile.
N-tert-amylacrylamide was recrystallised in warm benzene.
The white crystals have a mp.
910C(Lit.
91-920C)and the yield was 87%.
polymerization solvent, at 600C in the presence of AIBN
MBA
Aqueous solution containing NTA .
AM .
,MBA .
APS .
AcNa .
0, 0.
1, 0.
2, and 0.
, were prepared in methanol/water mixture.
The Fe3O4 NPs 50 mg were added during the polymerization by in situ .
After bubbling nitrogen for 30 min, the contents were placed in thermostatic water bath at 600C and the polymerization was conducted for 1 day.
After the reaction, the resulting Hydrogels were cut into pieces of 3-4mm long.
The extracted Hydrogels were dried in vacuum oven at 500C to constant weight for further use.
5 Characterization The FTIR analysis of the Nanocomposite hydrogel was carried out by FI-IR spectroscopy.
Scanning Electron Microscopy of hydrogels were Hitachi,model-JSM-5000 imaging mode at 30KV with varying levels of The catalytic reduction of MB dye was studied by UV-visible spectrophotometer.
Results and Discussion The synthesis of hydrogel was shown as scheme 3 Synthesis of Fe3O4 nanoparticles A solution was prepared by suspending 16.
FeCl3.
6H2O in 100 mL distilled water.
Similarly, another solution was prepared by suspending 6.
g FeCl2.
4H2O in 100 mL distilled water.
Both solutions were mixed in a glass beaker.
Then.
NH4OH was added dropwise to mixture formed by mixing of first two solutions of FeCl3.
6H2O
and FeCl2.
4H2O under continuous stirring at 70 AC till pH 10.
The resultant precipitate was filtered, washed, and dried.
Preparation Poly (N-tertamylacrylamideAeco-acrylamide/Sodium acrylat.
Fe3O4 Hydrogel Scheme : Poly (N-tert-amylacrylamide-coacrylamide / AcN.
Fe3O4 Hydrogel Free-radical crosslinking copolymerization was carried out in methanol /water mixture as the DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering Vol 3 .
, 2022 1 FT-IR spectroscopy The synthesized nanocomposite hydrogel was conformed by FT-IR spectroscopy and the characteristic values of functional groups are shown in Table 1.
Figure 2.
SEM image with EDAX of Ferrate nanocomposite hydrogel Figure 1.
FT-IR spectrum of Poly (N-tertamylacrylamide-co-acrylamide/AcN.
Fe3O4 Hydrogel Table 1.
Interpretation of IR spectra of Fe3O4 Nanocomposite Hydrogel 3489 cm-1 N-H of NTA and N-H stretching of AM 2923 cm-1 Methyl C-H symmetrical 1671 & 1735 cm C=O of NTA and AM 1110 cm-1 1266 cm-1 1392 cm-1 C-O stretching C-C stretching COO group of AcNa 1418 cm-1 C-N stretching of amide 719 cm-1 Fe-O stretching of Fe3O4 SEM analysis of Poly (N-tert-amylacrylamide-coacrylamide/AcN.
Fe3O4 Hydrogel SEM/EDAX micro analysis was employed to determine the constitution of the ferrate nanoparticles dispersed in the hydrogel matrix.
The EDAX spectrum.
Figure 2 shows well resolved peaks for Iron.
Carbon.
Oxygen and Sodium which are the elements present in the ferrate nanocomposite hydrogel.
The SEM image showed the Fe3O4 NPs were intercalated uniformly throughout the polymer matrix.
2 XRD Pattern of the Hydrogel XRD pattern of the hydrogel was shown in Figure 3, the peak at 2 value 20 having broad peak which indicate amorphous in nature .
The peaks at 20.
5, 30.
0, 50.
0, 55.
5 and 88.
2 2 are conforms the presence of Fe3O4 NPs in the polymer matrix.
3 Catalytic reduction of MB dye The catalytic reduction of methylene Blue dye molecules in aqueous solution by hydrogel is shown in Figure 4.
About 20 mL of 50 ppm MB solution was taken in a beaker and few drops of sodium borohydride along with the 0.
1g of nanocomposite hydrogel was added into the After 30 mins the dye solution are taken to UV-visible absorption study.
The absorption peaks shows the complete degradation of MB dye molecules in aqueous solution as shown in the Figure 5 .
DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering Vol 3 .
, 2022 of MB dye using nanocomposite hydrogel was conformed by UV-visible absorption study.
Acknowledgement The authors thank the IUAC .
New Delhi for support of the project work (Project No.
71345/2.
References