NMP Technology on Lube Extraction R&D Effort Towards

1. NMP Technology on Lube Extraction R&D Effort Towards Commercialization of Indigenous Technology Developed Jointly By Indian Institute of Petroleum Chennai Petroleum Corporation Limited Engineers India Limited

2. Introduction NMP technology aims to remove poly aromatics and other undesirable components from Lube Stock like LN,HN,BN,BS by using suitable solvent . Benefits from NMP Technology : • Improvement in viscosity index • Reduction of contaminants like sulfur and nitrogen compounds • Improvement in product color • Improvement in inhibitor response

3. High Selectivity Good Solvency Easy Recovery from hydrocarbon phase Good chemical and thermal stability Low vapor pressure to minimize energy Non Corrosive and non toxic Bio-degradability Low Cost Solvent Selection

4. Liquid SO2 -developed by Edeleanu(1907) Phenol - Licensed by Kellogg and Exxon (1930) ( No. of Plant in India : 1) Furfural - developed by Shell(1934) & Texaco ( No. of Plants in India : 1) N Methyl Pyrrolidone (NMP) -developed by Texaco(1965) & Exxon ( No. of Plants in India : 3) Solvent for Lube Extraction OH CH2 C=O CH2 N CH2 CH3 CH CH CH C-CHO O

5. Comparison of NMP, Furfural & Phenol OH CH2 C=O CH2 N CH2 CH3 CH CH CH C-CHO O

6. Comparison of NMP, Furfural & Phenol

7. Comparison of NMP, Furfural & Phenol

8. Comparison of NMP & Furfural

9. Comparison of NMP & Furfural Typical Utilities : Furfural Vs NMP

10. Comparison of NMP & Furfural Benefits of NMP Feed Stock : IN

11. Design of NMP Extraction Units

12. Steps in Process Design Feed Characterization Design of Extraction Section Design of Solvent Recovery Section for Raffinate Stream Design of Solvent Recovery Section for Extract Stream

13. Feed Characterization

14. Components in Lube Stocks Hydrocarbons Hetero Compounds Saturates Aromatics Paraffins Mono O Alkyl Naphthenes Di Poly S N Branched Paraffins

15. Objective : Generation of pseudo components Requires comprehensive experimental data Physical and Chemical characteristics Density, Pour Point, RI, Viscosity ,Total S,N,Wax Content, CCR, M.wt, Aniline point , ASTM Distillation(D1160),Carbon Distribution, %CA, %CN, %CP, RA,RN,%N+P,%A+S Phase Equilibria for LLE Continuous column studies IIP carried out Laboratory Study LLE study by in-house Simulator Prediction of phase equilibrium by UNIFAC Inputs for Feed Characterization

16. TypicalCompositions of Feed • Carbon no. changes from C15 to C50

17. EIL developed in-house simulator for generation of total heat & material balance for lube extraction unit Input for Simulator : Physical Properties of feed Liquid -Liquid Equilibria Water content in solvent Product specifications like VI of raffinate, desired raffinate yield etc to meet client’s requirement Flowsheet Simulation

18. Extraction Section

19. Solvent to Feed Ratio Temperature / Temperature Gradient of Extractor Water Content in Solvent Oil in Recycled Solvent Type of Extractor in Commercial Use Sieve Tray Extractor Packed Column RDC Design Parameters

20. Effect of Oil Content in Solvent on VI

21. Equipments Raffinate Recovery Section Raffinate Vacuum flash column Raffinate stripper Heat Exchangers Solvent Recovery Section

22. Equipments Extract Recovery Section LP,MP,HP Flash Columns Extract Vac. Flash Column Extract Stripper Heat Exchangers Solvent Recovery Section

23. NMP content in final raffinate - to be minimized Hydro carbon contents in extract – to be minimized Water content in solvent – to be appropriate for higher raffinate yield No. of flash columns in solvent recovery section for extract streams – to be optimized Optimization of heat exchanger network for energy saving Design Guidelines

24. Objective : To minimize solvent content in extract & raffinate R/D LP steam used as stripping medium Inert gas stripping Nitrogen may be used as inter gas Provides better operation Needs less energy Stripping Section

25. Solvent Drying Column to maintain desired water content in NMP Process variables : Water content in solvent Pressure of drying column Solvent loss through overhead Solvent Recirculation Section

26. Case Study ( NMP Extraction Unit- IOCL, Haldia) Licensed by EIL,IIP & CPCL

27. Design Capacity DAO : 125,000 TPA HN : 100,000 TPA IN :125,000TPA Turndown ratio : 50% Number of Trains : 1 Solvent : NMP Feed Characterization : By IIP Feed Temperature : 80 C Design Basis

28. Water injection at Extractor Bottom S/F ratio IN : 1.93 w/w HN :2.25 w/w BS :2.0 w/w Product Specifications : Raffinate Yield , VI & Pour Point IN : 52.4 wt%, 98, - 9.0 C HN :40.4 wt%, 96, - 9.0 C BS :56.1 wt%,95, - 6.0 C Design Basis – Continue ….

29. Process Flow Diagram

30. Process Flow Diagram

31. Process Flow Diagram

32. Key Operating Parameters

33. Plant was commissioned without any problem in 1999 and operation was found perfect . Plant is in continuous operation without any major problem since commissioning. As information available from IOCL , solvent loss may be one issue which needs to be taken care properly. Further work may be required for better operation of solvent recovery section and inter gas stripping may be considered as an alternative. Plant Performance & Future Work

34. Includes • Development of Basic Design & Engineering Packages for Extraction Unit • Detailed Engineering • Plant Commissioning • ( *with IIP and CPCL ) EIL’S (*) Offer for NMP Based Extraction Unit

35. Winner of CSIR National Award –2000

36. ACKNOWLEDGEMENTS We Express our Sincere Thanks to Indian Institute of Petroleum & Chennai Petroleum Corporation Limited for Technical Support in Development and Commercialisation of NMP Technology

37. Thank You