CSIR Leadership Conferenceoasis.csir.res.in/gum/fupld/mdocs/clc2012/CSIR-CS-IIP-LC_April 2012... · standalone units/ refineries ... Deoxygenation/Isomerization . Diesel . ... CSIR

WEL COME TO CSIR-IIP

CSIR-Indian Institute of Petroleum

CSIR Leadership Conference

26-28 April, 2012 Chandigarh

CSIR-IIP

Highlights of achievements in

last 5 years

CSIR Leadership Conference, Chandigarh, 26-28 April, 2012

Most Significant Achievements: 2007-12 CSIR-IIP

Technology Commercialized/ Transferred


•Pure Benzene •Gasoline:Sulphur <10ppm & Benzene <0.3%

CSIR-IIP Technology (Extractive Distillation)

CSIR-IIP Technology/Knowhow

Commercialization

NRL Dewaxing- Plant using CSIR-IIP Deoiling-Dewaxing Technology

Haldia SDU Revamp with IIP-EIL Know-how

Dewaxing-Deoiling Pilot Plant at CSIR-

IIP

Rs. 753.72 Cr Investment 50K TPA Paraffin wax 5K TPA µCrystalline Wax Technology by CSIR-IIP, PEDP by EIL with CSIR-IIP

Visbreaker Pilot Plant at CSIR-IIP

Internal-Soaker Technology for Visbreaking Unit at HPCL, Vizag

Solvent Extraction technique Energy Efficient Process Low cost Gr. II Lube Oil product

Plant capacity: 1.0 MMTPA CSIR-IIP Technology Engineering Package by EIL with CSIR-IIP

Fee received Rs135 Lakhs

Completion in July 2012 Test run in Aug. 2012

Production of Pure Benzene & US grade Gasoline from FCC Naptha

TIP in Progress Implementation in RIL, Jamnagar Installation, commissioning of Plant by RIL

CSIR-IIP Technology Commercialized CSIR-IIP Technology on Rerefining of used Lube Oil

Used oil Refined Product

Technolgy to M/s DeMenno Kerdoon, CA, USA

TIP & BDEP by CSIR-IIP Plant to start in early 2013 To be implemented in India


LPG SWEETENING CATALYST

CSIR-IIP Product Thoxcat ES Sweetening Catalyst

•Globally competitive. •Low cost •Less consumption •No further investment •Applicable in conventional & fibre-film sweetening processes

Catalyst Production Unit

Commercial Status: Used for LPG Sweetening in •FCC LPG Merox Unit of BPCL •LPG Merichem Unit of IOCL, Haldia •LPG Merox Unit of MRPL, Mangalore •LPG Merox Unit of BORL, Bina Trials runs with additives in •Sat LPG Merox Unit of RIL, Jamnagar in 2011 •Soon to be commercialized in RIL in 2012

•Patents: Foreign 06 Indian 03 •Publication: 03

Sweetening Unit

Licence Fee & 10% Royalty

CSIR-IIP Technology Commercialized


FCC

E X T R A C T I O N

LPG

GASOLINE

HCO

CLO

LCO

CLO

NMP

FEED

RAFFINATE

EXTRACT

CBFS / Mesophase Pitch

Upgradation of FCC Recycle Oil at HPCL

CSIR-IIP Pilot Unit

HPCL FCC Unit

FCC feedstock improvement Higher FCC product yield Co-production of premium quality CBFS

Rs.90.00 Cr/Annum Profit for Refinery

CSIR-IIP Technology Solvent Extraction Technique



Raw Materials: Neem, Ricebran, Karanja, Castor, Mahua, Linseed, Sugarcane etc.

Seed Oil

Chemical Processing

Developed Product

Soluble Cutting Oil

Biodegradable Soluble Cutting Oil

CSIR-IIP Technology Licensed to M/s EBLIPL, Coimbatore

100 MTPA Plant Commissioned in Feb.2012 Meets BIS Specs (IS 1115) For Ferrous & Non-Ferrous Metal Cutting

Technology Fees: Rs. 8.00 Lakhs + 5% Royalty Patent: IN 244501


Significant Achievements under Non-Plan Projects


Waste Plastics to Fuel & Petrochemicals

SCREW FEEDER

PYROLYZER

FEED (PE/PP)

FRAC

TIO

NAT

OR

GASES (C1-C5)

GASOLINE / DIESEL / AROMATICS

CATALYTIC REACTOR

RESIDUE

Diesel (~850 ml)

+ LPG

Gasoline (~700 ml)

+ LPG

Petrochemicals (~ 500 mL) +LPG

1 Kg waste (PE+PP)

Environment friendly solution to waste plastics disposal

Augment the supply of fuel and petrochemicals

Generate employment

SALIENT FEATURES • Exclusive production of either gasoline or

diesel or aromatics alongwith LPG from polyolefinic wastes (e.g. HDPE, LDPE, PP etc)

• Liquid fuel meet Euro III specifications • Simple, pollution free and environmental

friendly process • Estimated payback period for a 30 TPD plant ~

3 years

Lab scale (2006-2008) Waste plastics to value added hydrocarbons

Bench scale (Oct 2009-Dec 2011) Waste plastics to gasoline/diesel/aromatics

5 TPD pilot plant to be set up by GAIL Project management consultancy by IIP

BENEFITS

• Gasoline obtained from waste plastics

Plastics consumption in India (2010): ~10 MMT Plastic wastes in India (2010)*: ~15,000 TPD *source -CPCB


Demonstrated ULSD production at laboratory scale unit

Suitable for small scale standalone units/ refineries

Ready for Commercialization

Oxidant

Diesel fuel

OXIDATIVE DESULPHURIZATION OF DIESEL

ULSD Oxidation Extraction Adsorption

S< 10 ppmw Salient Features: • Mild operating conditions • less capital and operating • cost • No hydrogen, reduces GHG

emissions • Improves cetane index


SINTEF

Technology Development for Ultra Low Sulphur Diesel Production

Adsorbent Synthesis (SINTEF)

Process Flow Sheet Development (IIP)

Library Design (DOE)

Combi Testing

XRD

Data Analysis

Data Storage

Parallel Sample Isolation

MultiAutoclave (sample array)

Robotics

Adsorbent Screening (IIP)

16 16.2 16.4 16.6 16.8

17 17.2 17.4 17.6

mL

/ g

Volume of Diesel Treated per Gram Adsorbent up to 30 ppm

Sulphur BT Level

Adsorbents

A B

Ad-1001Adsorber

Ad-1002Adsorber

E-1008 A/B/C/DHDS FEED Effluent Exchanger

C-1002Reg Gas Recycle compressor

E-1009Reactor efflluentTrim cooler

E-1010AdsorberEffluent Trim cooler

F-1001/1002Furnace

AFC-1002ADS EffluentAir Condensor

D-1001/1002/1003Separator drum

P-1005Quench pump

D-1004Amine KO Pot

T-1002Amine Absorber

Swee

t pu

rge

gas

INDIAN INSTITUTE OF PETROLEUM

PROCESS FLOW DIAMGRAM FOR INTEGRATED HDS-ADSORPTION PROCESS FOR ULS DISEL PRODUCTION

Lean amine

Slip Streamto Claus unit

F-1001

C-1002

E-1010

Make-UpN2Air

Diesel feed (2000 ppm s)

DIESEL Feed(2000 ppm S)

Boiler feed water

AFC-1003

Rich amine

SourWater

T-1002

D-1001

E-1008 B

E-1008 A

E-1008 C

F-1002

P-1005

E-1009

1

AFC-1002

Desulphurised diesel

2

5

3

4

E-1008 D

AFC-1003 Regeneration gas Air Cooler

H2

40

320

P-1005Quench pump

15

16.8

332

17.8

18

6.4

14.4 E-1011

48

E-1011 Lean Amine Preheater

To flare

Pressure , kg/cm2,g

Temperature 0 C

E-1012

E-1012Reg.gas exchanger

•Developed vapor phase adsorptive desulphurisation process for diesel • S < 50 ppm •H2 requirement is 6 times lower •lower operating pressure •integration with existing hydrodesulphurisation •Adsorbent thermally regenerable

Indo-Norwegian Co-operation Programme

Novel low carbon emitting technologies for production of ultra low Sulphur Diesel

IIP

High through put combinotarial screening leading to novel sulphur selective adsorbents


CSIR-IIP Technology for Removal of SO2 from Flue Gas Streams

CSIR-IIP Process on Absorption

Pilot Plant by EIL with CSIR-IIP Knowhow •Generation of large databank

on solvents for SO2 removal • Development of thermally and chemically stable solvents

• 100 % slip over CO2

• MOU signed between CSIR – IIP, EIL and NRL • BDEP by CSIR-IIP & EIL • Commercialization at Numaligarh Refinery

Limited (NRL) & IOCL, Guwahati • Capacity: ~5000 Nm3/hr flue gas

Pilot Plant at EIL, New Delhi

CSIR-IIP Plant


CSIR-IIP Technology for gas removal by Absorption Process

CSIR-IIP Pilot Plant

Ready for Commercialization Jubilant Organosys Ltd Capacity : 6000 Nm3 per hr biogas

•Indigenous catalyst developed • Novel promoter •Much superior performance compare to commercial catalyst

CSIR-IIP Screening Unit

CO2 Removal

Ready for Commercialization

Chambal Fertilizer Ltd. Capacity : 450 MTPD of CO2 production

Large solvent databank solvents with improved characteristics Reduction in solvent regeneration energy requirement

H2S Removal


Significant Achievements under XI FYP Projects


Green jet fuel can match properties of petroleum derived Jet fuel. Increased demand for green jet due to CO2 legislation, energy security.

Light Gases Deoxygenation/Isomerization Diesel

Deoxygenation/Selective Cracking/Isomerization

Light Gases

Naphtha

Biomass Derived oil

Bio-Jet Fuel

Diesel Acid Gas Removal

Vegetable Oil

Reactor

Separator

H20

CO2

+ Gas OilMake up Hydrogen

Propane &Light Ends

Naptha or Jet

Diesel Product Capacity: 100 kg feed/day.

15 Liters of Bio-Jet Fuel supplied to Industrial Partners HPCL & IOCL

The Bio-Jet Fuel Meets all the Major Specifications for Aviation Fuel.

CSIR-IIP Pilot Plant

Publication: 15 (HIF:9.446, LIF: 2.791, AvIF: 4.56)

Patents: 3 Collaboration with Pratt & Whitney, Canada CSIR Leadership Conference, Chandigarh, 26-28 April, 2012

BIOETHANOL PRODUCTION FROM CELLULOSE AND STARCHY BIOMASS USING THERMOPHILIC MICROORGANISMS

1 Tonne SCB yields 206 L dry ethanol (from hexose stream) 22.5 kg yeast biomass (pentose sugar stream) 22.5 kg furfural (catalytic conversion of pentose

sugar stream) Recovery of ethanol by solvent extraction; reduces

the energy requirement Whole genome sequencing of thermophilic yeast

ethanologen Kluyveromyces sp. IIPE453 (collaborative work with CSIR-IGIB and TCGA))

fermentation at 500C

85 - 90% recovery of total sugar

dil. acid pretreatment followed by enzymatic saccharification

saccharification by novel amylase at elevated temperature

96% recovery of ethanol from fermentation broth by

solvent extraction

Thermophilic yeast Kluyveromyces sp.

IIPE453

MoU with Praj Matrix for Technology Development in Pilot plant & commercialization Patents: Foreign-5, Indian-2 Publication: 8 PhD: 3


For CO2/CH4 feed mixture CH4 purity exceeds 95 mol% CH4 Recovery > 85%

Adsorption Technology Development for CO2 Recovery from Biomass Pyrolysis / Gasification Off Gas

CSIR-IIP V S Processes

Gases H2, CO2, CO,

CH4, C2H4

Commercialisation Prospects Small scale Food/Agro Industries

•Highly selective adsorbent developed , superior to conventional adsorbents •Satisfactory Adsorbent performance with ternary feed mixtures

Designed a PVSA cycle with high performance in simple configuration

CSIR-IIP SINTEF Joint Project Collaboration with NTPC Tie-up with Monash Univ.

Patents:Foreign-1, Indian-3 Publications: 6 (Av IF=2.52) PhD: 2

CSIR-IIP’s Developed PVSA System


Biodegradable Lubricants

Raw Materials: Neem, Ricebran, Karanja, Mahua, Castor, Linseed, Sugarcane etc.

• Soluble Cutting Oil

• Transformer Oil

• Gear Oil

• Lithium Grease

• Hydraulic Oil

• 2 T Oil

Ecofriendly Additives • Extreme Pressure gear oil additives from

hyderogenated phospho-sulfurized cardanol • Additive Pack for Soluble Cutting Oil, 2T Oil, Gear Oil,

Hydraulic Oil, Lithium Grease and Transformer Oil

Key Significances: • Provides better Lubricity, Reduces break down period. • Completely biodegradable from agro-products. • Safe to use, no health hazards, no disposal problem • From Renewable source • High flash point, less volatile, food grade & non toxic • Compatible with mineral oil

Chemical Processing

Developed Product

End uses

Technology licensed Patents, Foreign:17 Indian: 2 Papers: 6


19

Modified alkyd resin development for value addition to Glycerol

The know how for production of modified alkyd resins using glycerol for various specialty end uses.

WSD: 0.78mm; Coefficient of friction: 0.02, Weld load:215kg

4 Ball Rig Test; Load:200kg

SEM of Ball after test

ATRP (initiator, methyl-2 chloropropionate; Ligand, N,N,N,N,N pentamethyl di-ethylene tri-amine; metal halide, copper chloride) in ratios 100:1:1:2

Glycerolmonomaleate

15 min., Stirring, N2 flushing (1:1 mole ratio)

Glycerol + Maleic acid

CoPolymers Am MMA

>30 polymers, optimized reaction

Coating (alkali,acid proof) Additive (aqu.& oil)

Product & process developed Ready for commercialization Dorf-Ketal

ATRP

•Publication: 06 •Patent: Indian 01 Foreign: 01


20

Important Chemical Intermediates from Glycerol

1,2 &1,3 propane diols

Under optimized condition, Product

Conversion > 85%

Product purity > 90% with pure

glycerol 80 % with

glycerol from biodiesel process

Cu-metal supported

catalysts found to be most

suitable

Butyl Ethers

99% conversion of glycerol with selectivity to

di- and tri-ethers greater than 95% was

obtained.

Commercial prospects:

Potential oxygenates to

diesel and biodiesel

reformulation.

Engine testing for emissions

2764/DEL/2011 dated

22.09.2011

0

1

10%GTBE/Diesel Diesel PM in

mg/

km

Compartive PM Emission

0

5

10

0 1 2 3 CO

in P

PM

Power KW

Comparative CO Emission

5%GTBE/Ga… Gasoline

GLYCEROL

40

50

60

Diesel 2.5% GTBE/Diesel 5% GTBE/Diesel Cet

ane

No

Cetane No Trends While Blending

GTBE


Engine Performance Studies

Evaluation of bio-fuels developed under the project for their suitability in advanced technology vehicles for desired performance and for meeting Indian mass emission norms

SEM Image of particulate from 10%bio-diesel/diesel Blend

Parameters Total Number Count/cc

Geometric Mean Diameter (nm)

Count Mean Diameter (nm)

Bio-Diesel

2.09E+08 42.87 60.99

Diesel 2.33E+08 57 69.88

Particulate size distribution measurements for Biofuels

Preliminary stability studies of Ethanol /Diesel Blends using Butanol as a Co- solvent

Optimization of Spray Characteristics of Butanol /Gasoline Blend (B10)

Evaluation of GTBE as Fuel Additive Preliminary stability studies of Ethanol /Diesel

Blends using Butanol as a Co-solvent Effect of biodiesel addition in diesel on nano size

particle distribution in the engine exhaust


Glimpses of CSIR-IIP Achievements(2007-2012)

No. of Technology Developed,Commercialized/Licenced: 12 No. of Paper Published: 180

No. of Patents; Foreign: 48 (filed & sealed) Indian: 31

Awards/ Recognizations:


Leader Ship and Excellence Award - OCEANTEX 2008 (Outstanding Achievement Award for R&D and Innovation) CSIR Technology Award-2009 Gold Medal from FICCI in DST-Lockheed Martin India Innovation Growth Programme on 20th May, 2010

CSIR Technology Awards – 2011 for “Business Development & Technology Marketing”

OceanTEX 2012 Leadership and Excellence Awards for the category of Outstanding Achievement in Research and Development


A long journey ahead

Thank You

Patents

Licensee

Catalyst Specifications


Commercial Status


Salient Features

Sweetening Unit

Product Name : Thoxcat ES Form : Liquid solution Color : Dark blue Odor : Odorless Specific Gravity @ 15/15 oC :1.06 ±0.02 Active ingredient, kg/bottle : 0.5(in 4.7 litres)

•Thoxcat ES catalyst is globally competitive. •Economical due to its low cost •Consumption is less for similar conversion •No investment will be needed for any plant modification •Applicable in conventional as well as fibre-film sweetening processes

The catalyst has been successfully tested in following units: •FCC LPG Merox Unit of BPCL •LPG Merox Unit of RIL, Jamnagar •LPG Merichem Unit of IOCL, Haldia •LPG Merox Unit of MRPL, Mangalore This had shown better performance than other catalyst being used earlier by them. BPCL Bharat Petroleum corporation Ltd (BPCL), Mumbai; Hindustan Petroleum Corporation Ltd(HPCL), Mumbai and Visakhapatnam, Chennai Petroleum Corporation Ltd (CPCL), Chennai and BORL, Bina are using this catalyst for LPG sweetening.

Granted : Total –9; USA – 2, UK – 2, France - 2, India – 3; Published : Germany – 2.

License for production and sale of this catalyst Thoxcat ES has been given to M/S Lona Industries Limited, Alta Bhavan, 532 Senapati Bapat Marg, P.O. Box No. 17006, Dadar, Mumbai-400028.


CSIR-IIP Product Thoxcat ES Sweetening Catalyst

Licenced to M/s Lona Industries Ltd, Mumbai


Trials runs with additives in •LPG Merox Unit of RIL, Jamnagar in 2011 •To be commercialized in RIL in 2012

Sweetening Unit

Licenced Fee & 10% Royalty


•Globally competitive. •Low cost •Less consumption •No further investment •Applicable in conventional & fibre-film processes

Commercial Status: Used for LPG Sweetening in •FCC LPG Merox Unit of BPCL •LPG Merichem Unit of IOCL, Haldia •LPG Merox Unit of MRPL, •LPG Merox Unit of BORL, Bina

FCC

E X T R A C T I O N

LPG GASOLINE

HCO CLO

LCO

CLO

NMP

FEED

RAFFINATE

EXTRACT

CBFS / Mesophase Pitch

•Patents: Foreign 06 Indian 03 •Publication: 03

Haldia SDU Revamp with IIP-EIL Know-how

Dewaxing-Deoiling Pilot Plant at CSIR-IIP

Production of Paraffin & Microcrystalline Waxes

CSIR-IIP Deoiling-Dewaxing

Technology

Numaligarh Refinery

(NRL) Wax Deoiling

Unit 50,000 TPA Paraffin Wax

5,000 TPA µCrystalline Wax

Rs. 753.72 Cr Investment

Technology Development & Basic Design Data generated by CSIR-IIP

PEDP by EIL with Technical support by CSIR-IIP

Licence Fee Rs. 2.16 Cr. & PEDP Fee Rs. 2.70 Cr

Plant going on-stream by Dec. 2013

Documents

CSIR Leadership Conferenceoasis.csir.res.in/gum/fupld/mdocs/clc2012/CSIR-CS-IIP-LC_April 2012... · standalone units/ refineries ... Deoxygenation/Isomerization . Diesel . ... CSIR