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SPS 5903SEMINAR RESEARCH PROPOSAL

Removal of Heavy Metal from aqueous solution by using Poly(Acrylonitrile-Acrylic Acid) AmidoximeMASTER OF SCIENCECHEMICAL ENGINEERING UPM

Name: Nur Amirah Binti Mohd ZahriMatric No.:GS39436Chairman: Prof. Dr. Luqman Chuah AbdullahInt. Members:Dr. Siti Nurul Ain Binti JamilDr. Mohsen Nourouzi MobarekehExt. Member: Dr. Sim Jia HueyPrepared by,

(Nur Amirah Binti Mohd Zahri)GS 39436Approved by,

(Prof. Luqman Chuah Abdullah)Chairman Supervisor ComitteeSPS 5903SEMINAR RESEARCH PROPOSALProcess FlowSynthesisModificationAdsorption & RegenerationRSM/WNNBET analysisCHNS, SEM & BET analysisOn goingNot Started yetPART 1PART 2PART 3PART 4

H2NOH

AcrylonitrileAcrylic Acid+Poly(Acrylonitrile-Arcylic Acid)+Hydroxylamine (Amidoxime)Scheme 1: The conversion of nitrile group to amidoxime group in Poly(Acrylonitrile-Arcylic Acid) Horzum et. al., 2012Introducing Arcylic Acid to AcrylonitrileIf only Homo-Poly(acrylonitrile)High polarityNitrile-nitrile dipolar interactiveNot porousWhen arcylic acid being added, polymer will becomeMore hydrophobicHigh in porousityPART 1: SynthesisRatio of Copolymer (Acrylonitrile:Arcylic Acid)Percentage of Yield (%)Homo-Polyacrylonitrile (Homo-PAN) 100:072.6697:364.1695:571.0093:772.1590:1062.88Speed of stir: 200 rpm, Temperature: 40oCTable 1: Calculated Data of Percentage YieldHomo-PAN (100:0) has the most high yieldWhen Arcylic Acid (AA) being added for the following ratio the yield drop Lower comonomer: degree dissociation high so yield become lowAs increase comonomer: degree dissociation low so yield increasingCertain level comonomer: decrease in the conc. in carboxylate ion more reactive toward the reaction initiating species R as well as to the radical growing polymer chain.Graph 1: Percentage of Yield Polymerization Synthesis

Introducing Hydroxylamine hydrchloride (Amidoxime group) to Poly(Acrylonitrile-Arcylic Acid)Only take place at nitrile groups to convert into amidoxime groupsHigh adsorption affinity to metal ions. Saeed et al 2008There is 4 different method have been tried to convert CN to C=N by using hydroxylamine Method 2 & 4 completely successful.Further the experiment with Method 2 because of:-simplicity of step compare to method 4simplicity of step compare to method 4Graph 2: Infrared Spectra (FTIR) of different method modificationFunctional GroupC = N

C = O

O H stretch

O H bend

N H2

N O

Frequencies Range (cm-1)1640-16701580 19003400 2400950-9103400-35001600-15301390-1300Method 11640.01640.03190.01-3190.01-Method 21642.031642.033332.65928.283332.651386.78Method 3- But CN (2243.41)1581.623358.15-3358.151581.62Method 41642.621642.623168.41-3168.411387.50Table 2: IR spectra for different modification method ANALYSISScanning electron Microscopy (SEM)BrunauerEmmettTeller (BET)Fourier Transform Infrared Spectra (FTIR)CHNS elemental analysisUnmodified : WaitingModified : WaitingUnmodified : CompletedModified : WaitingUnmodified : CompletedModified : WaitingUnmodified : CompletedModified : CompletedSEM analysis

100:095:597:390:1093:7

* 134.6nm* 177.9nm* 130.2nm* 158.6nm* 160.0 nm

* Average polymer bead sizeFTIR analysisGraph 3: Infrared Spectra (FTIR) of Poly(Acrylonitrile-Arcylic Acid) and Poly(Acrylonitrile-Arcylic Acid) Amidoxime for different ratio copolymerFunctional GroupC=N/C N

C = O

O H stretch

O H bend

N H2

N O

Frequencies Range (cm-1)1640-16702200-23001580 19003400 2400950-9103400-35001600-15301390-1300AMIDOXIME MODIFIED100:01642.761642.763326.11918.783326.111386.5497:31642.671642.673323.21922.433323.211386.6495:51639.151639.153197.59918.963458.981376.4093:71642.341642.343322.10915.343322.101386.1290:101643.441643.443331.90927.663331.901386.85UNMODIFIED100:02244.13-2932.73---97:32244.451732.162935.01---95:52244.811729.792933.70---93:72244.161729.362933.39---90:102244.981728.272934.70---Table 3: IR spectra for unmodified and amidoxime modifiedSampleCarbon (%)Hydrogen (%)Nitrogen (%)Sulphur (%)AnalysisCalculatedAnalysisCalculatedAnalysisCalculatedAnalysisCalculated100:063.5956.806.774.8624.5122.091.015.9797:361.2156.316.434.8724.0721.272.075.9395:559.8955.986.324.8720.9020.743.105.9093:763.2755.666.854.8721.1020.190.065.8790:1059.755.186.424.8819.3719.400.215.82CHNS analysisTable 4: CHNS Poly(Acrylonitrile-Arcylic Acid) Horzum, N., Shahwan, T., Parlak, O., & Demir, M. M. (2012). Synthesis of amidoximated polyacrylonitrile fibers and its application for sorption of aqueous uranyl ions under continuous flow. Chemical Engineering Journal, 213, 4149. doi:10.1016/j.cej.2012.09.114Saeed, K., Haider, S., Oh, T.-J., & Park, S.-Y. (2008). Preparation of amidoxime-modified polyacrylonitrile (PAN-oxime) nanofibers and their applications to metal ions adsorption. Journal of Membrane Science, 322(2), 400405. doi:10.1016/j.memsci.2008.05.062

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