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IMPACT™ Technology
A Greener Polyether Process
Jack Reese
Ken McDaniel
Robert Lenahan
Robert Gastinger
Mark Morrison
Polyurethanes
Presentation Overview
ƒ Introduction to Polyether Polyol Market and Applications
ƒ Polyether Polyols Chemistry
ƒ IMPACT™ Technology – Catalyst and Process
ƒ A Greener Polyether Process Technology
ƒ Summary
Polyurethanes
Introduction to Polyether Polyols
ƒ Main Application Area for IMPACT™ Technology is
Polyether Polyols for Polyurethanes.
ƒ Lower Molecular Weight (<10,000 Daltons) Polymers with
Terminal Hydroxyl Groups.
ƒ Starters for Polyols are Typically Propylene Glycol,
Glycerin, Sorbitol, etc.
ƒ Formed by the Catalytic Reaction of a Starting Polyol with
an Epoxide Containing Monomer.
ƒ Other Application Areas for Alkoxylation Technology
include Surfactants and various Functional Fluids.
Polyurethanes
Polyether Polyol Use in Polyurethanes
CH3
NCO
NCO
O
n
Long Chain
n > 8;
Short Chain
n < 8;
O
TDI
n
O
OH
Functionality =
2-6
n
Functionality =
2-8
Blowing Agent
MDI
NCO
O
O
OCN
O
Catalyst
HO
Additives
Polyether Polyols
Isocyanates
HO
Polyether Polyols:
Polyurethanes
R
H
N
O
O
Polyurethanes
R'
~ 40% of Polyurethane
~ 350 Different Varieties
Determine Unique Properties
Polyurethanes
World Consumption 1970 - 2010
(in mT)
Polyether Consumption ~ 4.6 mT or 10.2 billion lbs/yr
16
Steady growth at 4% (average) per year
14
2008:
11.6 mT
12
Forecast
10
8
6
4
2
0
1970
1975
Polyurethanes
1980
1985
1990
1995
2000
2005
2010
Polyurethanes
World Consumption by Application 2008
Others 18,5%
(e.g. TPU, Shoes,
RIM, Fibers)
Rigid Foam 25,5%
(Construction,
Insulation
Elastomers 5,5%
Adhesives and
Sealants 5,5%
Coatings 2,5%
Molded Foam 11,0%
(Automotive,Furniture)
Total: 11.6 Mio T
Polyurethanes
Source: Marketing-Dienste Dreger:
div. professional articel, Plastics 10-2008
BMS expansion and estimate
Traditional Polyether Process Chemistry
ƒ Polyether Polyols are made by ring opening polymerization
of an epoxide group onto a starter alcohol.
ƒ Main catalyst for the last 50 years is KOH.
R
OH
HO
OH
Starter
Glycerin as example
Polyurethanes
+
H2C
CH
O
R = CH2 for Propylene Oxide (PO)
R = H for Ethylene Oxide (EO)
KOH
Traditional Polyether Process Chemistry
ƒ Polyether Polyols are made by ring opening polymerization
of an epoxide group onto a starter alcohol.
ƒ Main catalyst for the last 50 years is KOH.
R
OH
HO
O- K+
+
H2C
CH
O
CH3
OH
HO
O
O- K+
Polymerizate or Crude Polyol
Polyurethanes
Traditional Polyether Process Chemistry
CH3
OH
O
HO
O- K+
PO / EO
PO
PO / EO
...
PO OH
O
PO
O
HO PO
...
PO O
...
Polymerizate or Crude Polyol
Contains between 0.2 to 0.4% KOH
Polyurethanes
PO O -K+
Traditional Polyether Process Chemistry
PO
...
PO OH
O
HO PO
...
PO O
O
PO
PO O- K+
...
Crude Polyol with 0.2 to 0.4% KOH
Work-up for K+ Removal
Neutralization
Distillation
Solvent Recovery
Purification
Polyurethanes
+ H2SO4
+ H2O
PO
...
PO OH
O
... PO O
O PO ... PO OH
-K2SO4 HO PO
-H2O
Final Refined Polyether Polyol
Containing less than 10 ppm K+
KOH Technology
ƒ Advantages
– Inexpensive catalyst.
– Wide range of products / Industry standard.
– Narrow molecular weight distribution.
ƒ Disadvantages
– Long reaction times.
– Need to remove catalyst (multi-step, energy intensive).
– Side reaction that reduces functionality at higher MW.
H2C
PO
O
H
C CH3
K+
Isomerization
OH
Allyl Alcohol
Polyurethanes
OH Allyl Alcohol
K+
OH
+ n PO / EO
n
Monol or unsaturation
Double Metal Cyanide (DMC) Catalysts
ƒ Zinc Hexacyanocobaltate, originally with glyme as ligand.
ƒ Invented in 1964 by General Tire.
ZnCl2 + K3 [Co(CN)6 ]
Zn3 [Co(CN)6 ]2 .8 H2 O.
Crystalline solid
Ligand = Glyme
Zn3 [Co(CN)6] 2. ZnX. Glyme
Amorphous/Crystalline
Catalysts
ƒ Advantages of glyme DMC catalyst over KOH:
– Lower by-product formation (50 – 70% reduction).
– Faster (shorter cycle times).
ƒ Disadvantages of glyme DMC catalyst over KOH:
– Cost (Much more expensive than KOH).
– Difficult DMC catalyst removal step.
Polyurethanes
IMPACT™ Catalyst
ƒ Developed in mid-1990s by ARCO Chemical (now part of Bayer).
ƒ Order of magnitude improvement in activity over glyme catalyst.
– Low catalyst levels possible – no catalyst removal required.
Faster Reactivity, Increased Selectivity, Simpler Process:
The Key to a Greener Technology
Reactivity
~ 1000x more
Reactive than KOH
More selective – little
to no by-product
KOH
Polyurethanes
IMPACT™
IMPACT™ Catalyst
ƒ Key invention was the novel combination of two ligands.
ƒ Amorphous catalyst structure.
ZnCl2 + K3[Co(CN)6]
XRD of IMPACT™
Ligand 1
Ligand 2
3500
Zinc Hexacyanocobaltate
3000
IMPACT™
IMPACT 3
H
R 1O
2500
Lin (Counts)
2000
Zn 3
1500
1000
O R2
Zn
Cl
CN
CN
Co CN
NC
NC CN
M a trix
3-
2
Amorphous/Crystalline
Catalyst
500
0
5
50
2-Theta - Scale
Zn3[Co(CN)6]2• ZnClY(OH)Z•L1•L2 • H2O
Polyurethanes
IMPACT™ Characteristics
Zn3[Co(CN)6]2• ZnClY(OH)Z•L1•L2•wH2O
PO
Low Molecular Weight
Starter
PG, Glycerin
Catalyst Inhibited
Reversible
-H2O
Inactive
Catalyst undergoes
activation in the
presence of starter
and oxide – MW
dependent.
PO
-H2O
High Molecular Weight
Starter
Very Active Catalyst
Heterogeneous
Particle Size Decreases
Industrial Challenge: Develop efficient process technology to use low
molecular weight starters (Gly or PG) directly.
Polyurethanes
IMPACT™ Process Technology
ƒ A more efficient process was required for commercial success.
ƒ Solution was provided in an inventive process named Continuous
Addition of Starter or CAOS.
Semi-batch process:
PO / EO
CAOS process:
PO / EO
Gly / PG
Product: 3000 MW
Product: 3000 MW
IMPACT™ Catalyst
Starter: 700 MW
made via KOH
low MW polyol heel
Starter: 1000 MW
made via IMPACT™
¾ CAOS is a more efficient process technology that eliminates the need for
KOH products as starters.
Polyurethanes
CAOS – Taking Advantage of Unique Kinetics
ƒ IMPACT™ Catalyst can tolerate low levels of glycerin or propylene glycol.
ƒ Conventional polymer kinetics predict broad polydispersity.
ƒ Example with 500 MW and 2000 MW as starter mix.
¾ KOH Catalysis as predicted by conventional polymer kinetics, Flory
500
750
1000
2000
2000
2250
2500
3500
Polyurethanes
CAOS – Taking Advantage of Unique Kinetics
ƒ Example with 500 MW and 2000 MW as starter mix.
¾ KOH Catalysis as predicted by conventional polymer kinetics, Flory
500
750
1000
2000
2000
2250
2500
3500
¾ IMPACT™ Catalysis
500
1000
1500
2000
2000
2000
2000
2000
“Catch-up Kinetics”
Polyurethanes
“Catch-up” Kinetics Demonstration
MW:
3600 2000
800
400
Weight Fraction
PO
Lower Molecular Weight Species React Preferentially
Providing a
Added
Narrow Polydispersity with Continuous Addition of Starter Technology.
100%
65%
45%
36%
26%
Starting Reactor
Contents
Polyurethanes
0%
Molecular Weight
PO
Addition
Utilizing Unique Kinetics to Optimize the Process
ƒ Highly active catalyst.
ƒ Ability to add low molecular weight starter during monomer feed.
¾ Ideal conditions for a continuous reactor system
Polyurethanes
Utilizing Unique Kinetics to Optimize the Process
ƒ Highly active catalyst.
ƒ Ability to add low molecular weight starter during monomer feed.
¾ Ideal conditions for a continuous reactor system
Continuous Product
400000
9000000
350000
8000000
Starter
EO, PO
Catalyst
300000
Tank Farm
GPC-Signal
250000
IMPACT
KOH
7000000
6000000
5000000
200000
4000000
150000
3000000
Reactor - CSTR
Cook out – PFR /
CSTR
100000
2000000
50000
0
100
IMPACT™ Continuous Technology
Polyurethanes
1000000
0
1000
10000
log(M)
Theoretical Distributions
100000
Polyether Process Technology Comparison
KOH, Semi-Batch
Starter
EO, PO
Catalyst
Solvent / Water
EO, PO
Salt
Tank Farm
Quality check
Starter
Reactor
Reactor
Neutralization
or Solvent Addition
IMPACT™, Continuous
Distillation /
Solvent
Recovery
Purification
Saving Areas:
Starter
EO, PO
Catalyst
• Energy / Steam
Tank Farm
Reactor - CSTR
Polyurethanes
Cook out – PFR /
CSTR
• Waste
IMPACT™ Technology – Energy Savings
Solvent / Water
KOH, Semi-Batch
EO, PO
Starter
EO, PO
Catalyst
Salt
Tank Farm
Quality check
Starter
Reactor
Reactor
Neutralization
or Solvent Addition
Starter
EO, PO
Catalyst
Distillation /
Solvent
Recovery
Purification
Energy Savings:
EO, PO
• Eliminate heat up and cool
down for every batch.
¾ Reduces steam and cooling
water.
Starter
Reactor
Polyurethanes
Reactor
IMPACT™ Technology – Energy Savings
KOH, Semi-Batch
Solvent / Water
EO, PO
Starter
EO, PO
Catalyst
Salt
Tank Farm
Quality check
Starter
Reactor
Reactor
Neutralization
or Solvent Addition
Distillation /
Solvent
Recovery
Purification
Energy Savings:
Solvent / Water
• Eliminate distillation of water
and/or solvent recovery.
Distillation / Solvent
Recovery
Polyurethanes
IMPACT™ Technology – Energy Savings
KOH, Semi-Batch
Starter
EO, PO
Catalyst
Solvent / Water
EO, PO
Salt
Tank Farm
Quality check
Starter
Reactor
Reactor
Neutralization
or Solvent Addition
Distillation /
Solvent
Recovery
Purification
IMPACT™, Continuous
Energy Savings:
• Steam and cooling water for batch process.
• Eliminate distillation of water and/or
solvent recovery.
Starter
EO, PO
Catalyst
• Potential to generate steam w/continuous
process.
Reactor-CSTR Cook out–PFR /
CSTR
Reductions – Steam = 99%, Electricity = 75% and
Cooling Water = 88%
Polyurethanes
IMPACT™ Technology – Waste Reduction
KOH, Semi-Batch
Solvent / Water
EO, PO
Starter
EO, PO
Catalyst
Salt
Tank Farm
Quality check
Starter
Reactor
Reactor
Neutralization
or Solvent Addition
Distillation /
Solvent
Recovery
Purification
Waste Reduction:
• No aqueous waste generated from
solvent removal and recovery.
Solvent / Water
Salt
• No solid waste generated from
catalyst removal.
Reductions – Solid waste = 100%, Aqueous waste = 98%
Polyurethanes
IMPACT™ Technology – Green Highlights
ƒ Case Study: Channelview, Texas facility – one KOH reactor and one
continuous reactor making similar products.
ƒ Easy conversion of existing KOH reactor to provide low cost capacity
increase while reducing process complexity.
ƒ Very consistent product quality – reliable on-line monitoring possible.
ƒ Little to no by-product formation – lower volatile organic compounds
(VOCs) in product.
ƒ Lower un-reacted oxide inventory in the reactor during the reaction
further reducing process safety risk.
ƒ Wastewater reduction of 75 million pounds per year.
ƒ Reduction of total energy consumption by 80 percent – this equates to a
yearly reduction of 54 million pounds of CO2.
Polyurethanes
Summary – IMPACT™ Technology A Greener Process
ƒ New Polyether Technology Developed and Commercialized.
– First Significant Change in 50 Years of Production.
– Technology Relies on Significant Catalyst Invention.
– Commercialization Realized with Significant Process Invention.
ƒ IMPACT™ Technology is a Greener Technology.
– Dramatic Reduction in Energy Use and CO2 Generation.
– Complete Reduction in Solid Waste.
– Significant Reduction in Aqueous Waste.
ƒ Development and Expansion of Technology Continuing.
–
–
–
–
Licensed to all Major Polyether Producers.
Approximately 50% of Bayer’s Polyether Volume has Developed Technology.
Recent Extension to High and Low Molecular Weight Polyether Grades.
Recent Extension to Incorporate the Use of a Renewable Based Starter (NOP).
ƒ Over 3 Billion Pounds of Polyether Produced based on IMPACT™ Technology.
ƒ Revolutionary Technology that Couples Positive Environmental Effects with
Increased Capacity that Optimizes Existing Assets.
Polyurethanes
Thank You for Your Attention
The authors wish to acknowledge the many scientists and engineers that have
contributed to the development and commercialization of the IMPACT™ Technology.
Polyurethanes
Polyurethanes