4 th InternatIonal ConferenCe on
advanCes In energy researCh
ICear-2013
IndIan InstItute of teChnology
MuMbaI (M.s) IndIa....
objeCtIve

2
Imidazolium

1-butyl-3-methylimidazolium
Chloride

3

Pyridinium

1-butyl-3-methylimidazolium
Bromide

Phosphonium

Ammoni...
4
Why Extractive desulfurization?
 In petroleum and hydrocarbon industries, various solvents such as ethers, amines,



...
Basic concept of Desulfurization

6
Characterization of ILs
FT-IR analysis of ionic liquids
1H-NMR and 13C-NMR analysis
Thermal Analysis
Conductivity Anal...
Results and Discussion
 Preparation of Model Fuel

A model liquid fuel with 500 ppmw sulfur (DBT as sulfur source)
was pr...
Effect of reaction time on DBT removal with IL

IL

Time (min)

S-content
(ppmw)

S-removal
(%)

Part. Coeff.
(KN)

5
214....
Effect of reaction temperature on S-removal with IL
IL

Temperature S-content S-removal Part. Coeff.
(OC)
(ppmw)
(%)
(KN)
...
Effect of S-compound on DBT removal

IL

Scontent
(ppmw)

Sremoval
(%)

Part. Coeff.
(KN)

DBT

169.55

66

1.94

BT

180....
Recycling of spent ILs without regeneration

No. of Cycle
IL
S-removal (%)
1
66
[BMIM]BF4
2
55.4
3
48.5
4
36
1
63.7
[BMIM]...
Desulfurization of Real Fuels using ILs

IL

Diesel/IL
(Mass Ratio)

Scontent
(ppmw)

Sremoval
(%)

Part.
Coeff.
(KN)

Gas...
Multistage Extraction Process

14
Conclusion

15
Highlights
 Imidazolium







16

based (ILs) were synthesized and employed as an
Extractant for S-removal.
Imidazo...
ApplicAtion of ils

17
Analytical Equipments Used

• Fourier Transform Infra Red (FTIR).
• Nuclear magnetic resonance (NMR)
• Differential Scanni...
Acknowledgement
s

CSIR
VNIT, Nagpur

19
20
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145 swapnil

  1. 1. 4 th InternatIonal ConferenCe on advanCes In energy researCh ICear-2013 IndIan InstItute of teChnology MuMbaI (M.s) IndIa. IONIC LIQUIDS:- ENERGY EFFICIENT GREEN SOLVENT FOR THE EXTRACTIVE DESULFURIZATION OF LIQUID FUELS Mr. Swapnil A. Dharaskar Research Scholar Under Supervision Dr. Kailas L. Wasewar & Dr. Mahesh N. Varma Department of Chemical Engineering Visvesvaraya National Institute of Technology (VNIT) Nagpur – 440010, Maharashtra, INDIA
  2. 2. objeCtIve 2
  3. 3. Imidazolium 1-butyl-3-methylimidazolium Chloride 3 Pyridinium 1-butyl-3-methylimidazolium Bromide Phosphonium Ammonium 1-butyl-3-methylimidazolium Tetrafluoroborate Sulfonium 1-butyl-3-methylimidazolium Hexafluorophosphate
  4. 4. 4
  5. 5. Why Extractive desulfurization?  In petroleum and hydrocarbon industries, various solvents such as ethers, amines,     a) b) c) d) 5 alcohols and other volatile organic compounds have been used for the options like extraction, absorption, azeotropic distillation etc. These solvents have their own limitations in terms of environmental issue, recycle ability, etc. which can be overcome by the use of ionic liquids as green solvent. Among theses EDS seems more eye-catching because it does not require hydrogen and catalyst and its operation conditions is mild. Moreover, it does not alter the chemical structures of the compounds in fuel oils and extracted S-compounds can be reused as raw materials. A good extractant much have the following attributes:Good extractive ability for S-compounds. Free of contamination to the fuels. Non-toxicity, and environmental benignity. Stability for repetitive use
  6. 6. Basic concept of Desulfurization 6
  7. 7. Characterization of ILs FT-IR analysis of ionic liquids 1H-NMR and 13C-NMR analysis Thermal Analysis Conductivity Analysis Solubility Analysis Viscosity Analysis 7
  8. 8. Results and Discussion  Preparation of Model Fuel A model liquid fuel with 500 ppmw sulfur (DBT as sulfur source) was prepared in n-Octane. Similarly, the model liquid fuels were prepared by dissolving BT, T, and 3-MT individually in n-Octane respectively. Actual diesel and gasoline with total sulfur content of 385.13 and 180.79 ppmw respectively were used.  Effect of Reaction Time on S-removal  Effect of Reaction Temperature on S-removal  Effect of S-Compound on S-removal.  Recycling of spent ILs without Regeneration.  Desulfurization of Real Fuels using imidazolium IL 8
  9. 9. Effect of reaction time on DBT removal with IL IL Time (min) S-content (ppmw) S-removal (%) Part. Coeff. (KN) 5 214.55 57 1.33 [BMIM]BF4 10 199.05 60.2 1.51 20 184.55 63 1.71 30 170.05 66 1.94 5 223.55 55.3 1.24 [BMIM]PF6 10 209.55 58 1.39 20 194.05 61.2 1.58 30 181.5 63.7 1.75 Temperature = 30OC, Mass ratio of model fuel/IL = 5:1, Extraction time = 30 min. Initial sulfur concentration = 500 ppmw. 9
  10. 10. Effect of reaction temperature on S-removal with IL IL Temperature S-content S-removal Part. Coeff. (OC) (ppmw) (%) (KN) 20 198.5 60.3 1.52 [BMIM]BF4 25 179.05 64.2 1.79 35 165.05 67 2.02 45 224.55 55 1.22 55 263.55 47.3 0.89 20 213.05 57.4 1.35 [BMIM]PF6 25 200.05 60 1.5 35 171.5 65.7 1.92 45 249.05 50.2 1.0 55 279.55 44 0.79 Temperature = 30OC, Mass ratio of model fuel/IL = 5:1, Extraction time = 30 min. Initial S-concentration = 500 ppmw. 10
  11. 11. Effect of S-compound on DBT removal IL Scontent (ppmw) Sremoval (%) Part. Coeff. (KN) DBT 169.55 66 1.94 BT 180.49 63.9 T 231.09 3-MT [BMIM]BF4 S-Compound 260.30 IL S- content (ppmw) S-removal (%) Part. Coeff. (KN) 174.09 65.2 1.87 1.77 210.39 57.9 1.37 53.8 1.16 250.19 49.9 0.99 47.9 0.92 285.79 42.8 0.75 [BMIM]PF6 Temperature = 30OC, Mass ratio of model fuel/IL = 3:1, Extraction time = 30 min. Initial sulfur concentration = 500 ppmw. Reactivity sequencing was DBT > BT > T > 3-MT. 11
  12. 12. Recycling of spent ILs without regeneration No. of Cycle IL S-removal (%) 1 66 [BMIM]BF4 2 55.4 3 48.5 4 36 1 63.7 [BMIM]PF6 2 53.4 3 45.2 4 31 Model fuel = (n-Octane + DBT), Mass ratio of model fuel/IL = 5:1, Temperature = 30OC, Extraction time = 30 min, Initial S-concentration = 500 ppmw. 12
  13. 13. Desulfurization of Real Fuels using ILs IL Diesel/IL (Mass Ratio) Scontent (ppmw) Sremoval (%) Part. Coeff. (KN) Gasoline/IL (Mass Ratio) S-content (ppmw) Sremoval (%) Part. Coeff. (KN) [BMIM]BF4 5:1 210.31 45.4 0.83 5:1 70.2 61.1 0.61 225.19 41.5 0.71 90.3 50 1.0 [BMIM]PF6 Temperature = 30OC, Extraction time = 30 min, Initial S-concentration of diesel and gasoline = 385.13 and 180.79 ppmw.
  14. 14. Multistage Extraction Process 14
  15. 15. Conclusion 15
  16. 16. Highlights  Imidazolium      16 based (ILs) were synthesized and employed as an Extractant for S-removal. Imidazolium Ils can be used as energy efficient green material for EDS of liquid fuels, mainly with regards to those S-compounds that are very complex to remove by common hydrodesulfurization (HDS) technique. The spent IL could be reused for four times with a slight decrease in activity. Enormous saving on energy can be achieved by use of IL in process. This work could be present a new alternative for extractive deepdesulfurization of liquid fuels. The EDS method could be option for environmentally benign method for deep desulfurization.
  17. 17. ApplicAtion of ils 17
  18. 18. Analytical Equipments Used • Fourier Transform Infra Red (FTIR). • Nuclear magnetic resonance (NMR) • Differential Scanning Calorimetry (DSC). • Thermogravimetric Analysis (TG/DTA). • Thermo-scientific Total Sulfur Analyzer (TS-3000). • Inductively coupled plasma-AES • X-ray fluorescence spectrophotometer (XRF) • UV visible Spectrophotometer. • Gas Chromatography with mass spectometry (GC-MS) High Pressure Liquid Chromatography (HPLC). 18
  19. 19. Acknowledgement s CSIR VNIT, Nagpur 19
  20. 20. 20

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