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Metal Organic Frameworks (MOFs) are novel materials with extremely high surface area (ca. 1000-5000 m2 g-

1), 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).

SUMMARY

OBJECTIVES

EXPERIMENTAL SECTION

• Degradation of Polystyrene (PS)

Virgin polystyrene(PS) or Styrofoam was obtained from discarded package. Thermo gravimetric Analysis (TGA) of

polystyrene was carried out using TGA-DTA analyzer for different heating rates in presence and absence of air.

Then a mixture of polystyrene and MOF was taken in TGA-DTA analyzer and thermo gravimetric studied were

carried out by varying following parameters.

Different type of MOF

Varying the heating rate

Changing the quantity of MOF

RESULT & ANALYSIS

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 Fe-

BDC, where the maximum degradation is about 12.3%.

• PS with Zn-BDC has shown about 50% degradation with

temperature difference of 65oC.

• PS with Pb -BTC has shown the highest degradation of 69.3%

with a temperature difference of 82oC.

EXPERIMENTAL SECTION • Synthesis of MOF catalysts.

Cu-BTC (or, HKUST-1)

Cu (NO3)2 + benzene tri-carboxylic acid (BTC) Cu-BTC (or, HKUST-1)

Zn-BDC (or, MOF-5)

Zn (NO3)2 + benzene di-carboxylic acid (BDC) Zn-BDC (or, MOF-5)

Fe-BDC (or, MIL-53(Fe))

FeCl3 + benzene di-carboxylic acid (BDC) Fe-BDC (or, MIL-53(Fe))

Pb -BTC

Pb(NO3)2 + benzene tri-carboxylic acid (BTC) Pb-BTC

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

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.

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

Department of Chemical Engineering, National Institute of Technology Rourkela, Odisha, India

Corresponding Author Email Address: chowdhuryp@nitrkl.ac.in

Prince George , Pradip Chowdhury*

Catalytic degradation of polystyrene using Metal organic frameworks

CONCLUSION

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Cu -Pure methanol

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Fe Fe

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MOFs AS CATALYSTS Cu-BTC Zn-BDC Fe-BDC Pb -BTC

Breakdown temperature (oC) 275 400 380 400

Experimental Temperature (oC) 250 350 300 350

MOFs AS CATALYSTS Cu-BTC Zn-BDC Fe-BDC Pb-BTC

Lower temperature Limit (oC) 150 125 75 50

Upper Temperature Limit (oC) 275 400 380 400

Temperature range under analysis (oC) 150-250 125-350 75-300 50-350

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CuBTC-PS

FeBDC-PS

ZnBDC-PS

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PbBTC

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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

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

A B

C D

Figure 3: TGA graph of MOFs

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.

Fe-BDC and Pb-BTC , Beyond 380oC and 400oC the structure

collapses for Fe BDC and Pb-BTC respectively.

Table 1: Breakdown temperature of MOFs Table 2: Temperature of MOFs taken under study for calculation of

effective degradation of polystyrene

Figure 4: Degradation of PS with/without MOFs

• 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.

ACKNOWLEDGEMENTS

• We acknowledge Department of Metallurgy and Materials engineering, National Institute of Technology Rourkela for

characterization.

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