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SUMMARY
Metal Organic Frameworks (MOFs) are novel materials with extremely high surface area (ca. 1000-5000 m2 g1),
uniform pore size distribution, tunable matrices (depending on newer synthesis strategies) classified under
Class IV co-ordination polymers. Three conventional metal organic frameworks viz. Cu-BTC (or, HKUST-1), Zn-BDC (or, MOF-5) and Fe-BDC were used as catalyst for the study. Additionally, an entirely new hybrid structure viz. Pb -BTC was synthesized and its effectiveness in degrading polystyrene was also studied. The polystyrene degradation performances of the MOFs were found to be in the decreasing order of Pb BTC>Zn-BDC>Fe-BDC>Cu-BTC. Notwithstanding their instability at high temperatures, MOFs had shown good catalytic performance in degrading polystyrene within their stipulated temperature limit (~250-325oC).
OBJECTIVES
FeBDC 20 CuBTC ZnBDC PbBTC 15
Synthesis of above mentioned metal organic frameworks (MOFs) ;Cu-BTC (or, HKUST-1), Zn-BDC (or, MOF-5) and Fe-BDC. Characterization of MOFs using SEM,XRD & BET surface area analysis ;Comparing the obtained results with literature data. Carrying out TGA of virgin Polystyrene sample, MOFs and Mixture of MOF plus Polystyrene. Determining Percentage degradation of Polystyrene with the limited temperature range. Evaluating the best MOF as catalyst
Weight loss (mg)
Highlights of Figure 3 Cu-BTC Range 25-125oC : Weight loss is purely due to removal of moisture and trapped solvent. Range 125oC to 275oC :Horizontal plateau, weight remains fairly constant. Range > 275oC : Cu-BTC structure collapses. Zn-BDC Range of 25-150oC : Weight loss is purely due to removal of moisture and trapped solvent. Range 150oC-400oC :Weight loss remained largely stable. Range> 400oC :Zn-BDC structure collapses.
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EXPERIMENTAL SECTION
Synthesis of MOF catalysts. Cu-BTC (or, HKUST-1) Cu (NO3)2 + benzene tri-carboxylic acid (BTC) Zn-BDC (or, MOF-5)
Figure 3: TGA graph of MOFs
Fe-BDC and Pb-BTC , Beyond 380oC and 400oC the structure collapses for Fe BDC and Pb-BTC respectively.
Cu-BTC (or, HKUST-1) Zn-BDC (or, MOF-5) Fe-BDC (or, MIL-53(Fe)) Pb-BTC
MOFs AS CATALYSTS MOFs AS CATALYSTS Breakdown temperature (oC) Experimental Temperature (oC) Cu-BTC 275 250 Zn-BDC 400 350 Fe-BDC 380 300 Pb -BTC 400 350 Lower temperature Limit (oC) Upper Temperature Limit (oC) Temperature range under analysis (oC)
Zn (NO3)2 + benzene di-carboxylic acid (BDC) Fe-BDC (or, MIL-53(Fe)) FeCl3 + benzene di-carboxylic acid (BDC) Pb -BTC Pb(NO3)2 + benzene tri-carboxylic acid (BTC)
Table 2: Temperature of MOFs taken under study for calculation of effective degradation of polystyrene
1 PS
The solution was then transferred into Teflon- lined autoclave, which was heated at prescribed temperatures. The reaction products were cooled to room temperature, and the solid obtained were collected by
Degradation (x)
0.9
Highlights of Figure 4 From Table 1 & 2 ,the reaction temperature range can be determined so as to prevent the degradation of MOFs. PS with Cu-BTC has shown least degradation followed by FeBDC, where the maximum degradation is about 12.3%. PS with Zn-BDC has shown about 50% degradation with temperature difference of 65oC.
0.8
PbBTC-PS
centrifugation. The crystals were washed with suitable solvents, dried and stored at room temperature. All the synthesized MOFs were characterized using standard characterization techniques e.g. Scanning Electron Microscopy (SEM), Thermo gravimetric Analysis (TGA), Powder X-ray Diffraction Analysis (PXRD) and BET Surface Area Analysis.
0.4
0.3
0.2
B
Intensity
Intensity
0.1 50 700 600 100 150 200 250 300 Temperature (C) 350 400 450 500 550
PS with Pb -BTC has shown the highest degradation of 69.3% with a temperature difference of 82oC.
A
Cu -Pure methanol
B
Fe Fe F e
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CONCLUSION
Degradation of polystyrene was found to be highest using Pb -BTC followed by Zn-BDC. Using MOFs the degradation temperature of polystyrene was lowered down ,thereby reducing energy expenditure. Recoverability of MOFs after the degradation process was possible , the process can be economic after optimization.
25 35 Two Theta Angle
D
Intensity
10
20
30
40
50
15
1600 1400 1200 1000 800 600 400 200 0 5 15 25 Two Theta angle 35 45
600
ACKNOWLEDGEMENTS
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Figure 1: SEM images of MOFs :(A) Cu-BTC (or, HKUST-1) (B) Fe-BDC (or, MIL-53(Fe)) (C) Zn-BDC (or, MOF-5) (D) Pb -BTC
RESEARCH POSTER PRESENTATION DESIGN 2012
Figure 2: PXRD data of MOFs :(A) Cu-BTC (or, HKUST-1) (B) Fe-BDC (or, MIL-53(Fe)) (C) Zn-BDC (or, MOF-5) (D) Pb -BTC
We acknowledge Department of Metallurgy and Materials engineering, National Institute of Technology Rourkela for characterization.
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