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INNOVATIVE EXTRACTION PROCESSES FOR CHALLENGING FEED-STOCKS. Indian Institute of Petroleum (Council of Scientific & Industrial Research ) Dehradun. SYMPOSIUM ON SOLVENT EXTRACTION REVISITED FEBRUARY 5 TH – 6th , 2010 IIChE (NRC) Auditorium NEW DELHI-INDIA. Aromatic Extraction.

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indian institute of petroleum council of scientific industrial research dehradun

INNOVATIVE EXTRACTION

PROCESSES FOR CHALLENGING FEED-STOCKS

Indian Institute of Petroleum (Council of Scientific & Industrial Research )Dehradun

SYMPOSIUM

ON

SOLVENT EXTRACTION REVISITED

FEBRUARY 5TH – 6th , 2010

IIChE (NRC) Auditorium

NEW DELHI-INDIA

aromatic extraction
Aromatic Extraction
  • Extraction Step

Removal of Aromatics

Recovery of Aromatics

Capacity

Selectivity

Pure BTX Production

FGH/SK/ATF/LOBS Production

Innovations Required

  • Solvent Recovery Step : Distillation
  • Limitations of conventional scheme
  • Overlapping of boiling point of feed-stock
  • & solvent
  • High level of impurities in feed stock
slide3

Examples

  • De-aromatization of Middle distillate by using re-extraction
  • Pure BTX from Straight Run Naphtha
middle distillate de aromatization
Middle Distillate De-aromatization
  • Trend towards increasing use of hydroprocessing
  • Not attractive for small refineries as requires high capital & operating expense
  • Loss of valuable aromatics
  • Search for alternative to hydrotreatment
  • Solvent extraction already established for naphtha fraction and Lube fraction
  • Extended to Middle Distillates
kerosene de aromatization using sulfolane based extraction
Kerosene De-aromatization using Sulfolane Based Extraction

Sulfolane Technology developed jointly with EIL and HPCL

Demo was given to IOCL on ATF pilot plant at HPCL, mumbai

Process Package along with EIL was submitted to IOC Digboi

limitations of sulpholane based extraction technology
Limitations of Sulpholane Based Extraction Technology

Utilities required were high due to use of distillation step for the solvent recovery

Further work was initiated at IIP to improve the solvent recovery process

  • RE-EXTRACTION
  • A novel approach for solvent recovery
re extraction technology
Re-extraction Technology

Replacement of energy intensive distillation step by using reverse extraction

High capacity solvent like NMP can be used in spite of boiling point overlap with feedstock – No distillation

Re-Extraction Solvent

Low Boiling Hydrocarbon Stream– Low energy required for separation from aromatics

like dissolves like
Like DissolvesLike

Aromatics in Feed

LPS + Aromatics

Saturate in feed

Extraction solvent

Re-Extraction Solvent

Re-extractor

Extract Phase

LPS

Lean Solvent

slide10

FLOW SHEET WITH RE-EXTRACTION

AROMATIC EXTRACT

TOP PHASE

LEAN SOLVENT

WATER

RE-EXT COL.

EXTN. COL.

SEC. SOLV. REC.

EXT- WASH COL.

FEED

WATER + NMP

EXT PHASE

SEC-SOLVENT

FURNACE

FUEL

DEAROM. RAFFINATE

RE-EXT COL BOTTOM

WATER

SOLV REC COL.

WATER

RAFF WASH COL.

LEAN SOLVENT

RAFFINATE

PHASE

WATER + NMP

challenges with given feed stocks

Challenges with Given feed-stocks

Three different feed-stocks of different boiling range

Conventional scheme with single solvent not feasible –

Boiling point overlap

Re-extraction with NMP using blocked out mode operation is an alternative

de aromatization in block out mode
De-aromatization in block out mode

Solvent

EXTRACTION UNIT

Heavy

Naphtha

De-aromatized

Heavy Naphtha

De-aromatized

Kero-fractiom

Kero

De-aromatized

Gas Oil

Gas

Oil

experimental studies
Experimental studies
  • Detailed experimental studies have been carried out with feedstock provided by Guwahati Refinery
    • Feed stocks analysis
    • Single stage LLE data
    • - Extraction
    • - Re-extraction
    • Continuous column studies for extraction and

re-extraction steps

  • Total number of data point generated = 175
slide17

Typical Experimental Results

Raffinate and extract produced met

the desired specifications

simulation and modeling
Simulation And Modeling
  • Feed Characterization (Model Hydrocarbons)

GC & GC MS Hydrocarbon type analysis

  • Prediction of LLE Based on UNIFAC
  • Development and Simulation of Process Flow sheet Using ASPEN PLUS
  • Optimization of Heat Integration and Operating Parameters to Minimize Utility Requirements
model hydrocarbons representing gas oil

Hydrocarbon Rep. Model Structural Mol. B.P.

Type Hydrocarbons Formula Formula oC

CH3(CH2)4CH3

C16H34 287

C20H40 351

C12H22 239

C14H22 264

C16H14 306

C13H14 274

C14H14 274

C13H10 297

C15H30

C2H5

Model Hydrocarbons Representing Gas Oil

C8H17

Paraffins n-Hexadecane

Non Condensed n-Pentadecyl

Cycloparaffins Cyclopentane

Condensed Bicyclohexyl

Cycloparaffins

Alkyl Benzenes n-Octyl Benzene

Indanes & 1-n-Hexyl 1,2,3,4

Tetralins Tetrahydro

Naphthalene

Diaromatics 1-n-Propyl

Naphthalene

Bi-phenyls 1,1-Diphenylethane

Fluorenes Fluorene

C6H13

C3H7

C2H5

summary de aromatization of middle distillate
Summary: De-aromatization of Middle Distillate
  • Re-extraction Technology is available for de-aromatization of petroleum fractions of different boiling ranges
  • Process package for similar application is already completed
background
Background
  • Huntsman Petrochemicals Ltd., approached IIP for revamp of their NMP unit
  • Revamp involved changing the feed from Reformate to Straight Run Naphtha to produce pure BTX and de-aromatized Naphtha as cracker feed
    • To increase feed-product differential costs
    • To increase the Naphtha cracker capacity and performance
improvement in naphtha cracker performance
Improvement in Naphtha Cracker Performance

Conventional Naphtha Cracking

Dearomatized Naphtha Cracking

C2/C3 Olefins

Paraffinic Naphtha

~10% aromatics

CRACKER

C2/C3 Olefins

Cracker

Paraffinic Naphtha

~10% aromatics

ARU

Pure B T & X

  • ~10% capacity addition can be obtained in the Cracker
  • Off spec cracker naphtha feeds can be used
  • Improvement in economic due to production of pure BTX
challenges to produce pure btx from sr naphtha
Challenges to produce pure BTX from SR Naphtha
  • Technologies for production of pure BTX from high aromatics feed stocks already established
  • Conventional feed stocks are rich in aromatics and low in naphthenes
  • Proposed feed stock : Naphtha
    • Aromatics content low (~10 wt.%)
    • Ratio of aromatic to naphthenes less than 1 (Higher Naphthenes)

Difficult to produce pure aromatics

without innovations

simplified process flow sheet for the production of pure aromatics
SIMPLIFIED PROCESS FLOW SHEET FOR THE PRODUCTION OF PURE AROMATICS

SOLVENT RECOVERY

RAFFINATE WASH

STRIPPER

EXTRACTOR

RAFFINATE

EXTRACT BENZENE

FEED

SOLVENT REGENERATOR

effect of carbon number and hc type on separation with solvent
Effect of carbon number and HC type on separation with solvent

Relative solubility

Relative volatility

Separation of naphthlenes is comparatively difficult by distillation

Stripper is limiting

extract purity improvement
Extract Purity Improvement

For achieving targeted purities of aromatics various combinations of the operating variables were tried:

  • Different S/F in the extractor
  • Use of different backwash streams along with existing backwash stream
  • Use of water as antisolvent
  • Use of secondary solvent
continuous column extraction runs with straight run naphtha at 40 c
Continuous column extraction runs with straight run naphtha at 40 °C
  • Back wash : Benzene Rich C6 cut
  • S/F : 3.0 w/w
  • Feed : S R Naphtha with 10% aromatics
  • Solvent : NMP with water
processing of straight run naphtha
Processing of Straight Run Naphtha

Composition, wt.%

P-65.83

N-31.60

A-2.57

Raffinate

Water

P-63.4

N-25.7

A-10.9

Solvent

Naphtha

EXTRACTOR

BW + recycle

P-16.5

N-2.2

A-81.3

Pentane

Extract

simulation and modeling of btx unit
Simulation And Modeling Of BTX Unit
  • Required modified interaction parameters for naphthenes and solvent
  • Large Number of LLE data with naphthenes ( Model HC) and solvent were generated which were not required for conventional system, for simulation studies
  • Simulation of Process Flow sheet Using ASPEN PLUS
plant simulation diagram
Plant simulation Diagram

Closed loops Simulation: Results gives us the confidence that data are correct and well fitted for real plant operation

btx quality achieved
BTX Quality Achieved
  • Solvent contamination : 1ppm
  • Non-aromatic content (based on normal boiling point)
    • bp<110 °C : 700 ppm wt/wt in benzene fraction
    • 110 °C<bp<136 °C : 2000 ppm wt/wt in toluene fraction
    • 136 °C<bp<138 °C : 3000 ppm wt/wt
    • in ethyl benzene fraction
    • 145 °C<bp : 5000 ppm wt/wt

in remaining fraction

process economics
Process Economics
  • The concept & economics of integrating Cracker with Straight Run Naphtha dearomatization was published in April 2007 issue of Hydrocarbon processing much after our work
  • The author studied two types of off spec. Naphtha for integrating dearomatization and cracking on a cracker
  • The payout period was found to be ~0.8 year
iip technology for pure btx from s r naphtha
IIP Technology for pure BTX from S R Naphtha

Outcome

Technology successfully developed and demonstrated on lab scale

Plan for retrofitting the above in the existing unit was also provided to the client in UK

slide38

THANK YOU

www.csir.res.in

www.iip.res.in