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P. I. in the UK:
PIN, PIG and OBRs
Adam Harvey
Professor of Process Intensification
Process Intensification Group
Chemical Engineering & Advanced Materials
Newcastle University Zeton BV, 7th November 2012
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“P.I.” Process Intensification
“The strategy of making dramatic*
reductions in the size of process plant
items by re-examining the fundamentals
of their heat and mass transfer”
*at least an order of magnitude
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Before: Current Chemical Process
Large
Smelly
Dirty
Dangerous
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After
Smaller
Leaner
More efficient
Reduced Emissions
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P. I. in the UK: PIN
“PIN” the Process Intensification Network. Managed by:
Prof David Reay Heriot Watt University
Prof Colin Ramshaw Cranfield University
Prof Adam Harvey Newcastle University
21st Meeting: March 2013
~300 on the mailing list: industry, academia, UK and
overseas
EPIC conference in Manchester 2011 (with the IChemE)
Email [email protected] or [email protected] to join
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P. I. in the UK: PIN
2nd Edition just
completed
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Process Intensification Group [PIG]
5 academic staff:
Adam Harvey (OBRs, biofuels)
Kamelia Boodhoo (SDRs, polymerisation)
Jonathan Lee (RPBs, carbon capture)
David Reay (heat pipes)
Sharon Orta (algae, fuel cells)
5 research associates/visitors
18 PhDs
http://pig.ncl.ac.uk
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PIG Activities
Technologies
Oscillatory Baffled Reactors (OBRs)
Spinning Disc Reactors (SDRs)
Rotating Packed Beds (RPBs)
Heat Pipes
Reactive Extraction (RE)
Microreactors: catalytic plate reactors
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PIG Activities
Application Areas Technologies
High throughput screening OBR
Heterogeneous Catalysis
i. Catalytic cracking for biofuels
ii. Solid catalysts for biodiesel
ii. OBR
Crystallization SDR, OBR
Biofuels & biorefining OBR, RE
Polymerisation SDR
Thermal management Heat Pipes, Heat pumps, Organic
Rankine Cycles
Bioprocessing SDR
RPB
CO2 Absorption RPB
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Biofuel Research Projects
1. Reactive Extraction (Biodiesel) 1. Rapeseed [PhD] Malaysian Govt
2. Jatropha + other inedible [PhD] UKIERI
3. Algae [PhD] Nigerian Govt.
2. Oscillatory Baffled Reactors: 1. Bioethanol production [PhD] Nigerian Govt
2. Biobutanol production [PhD] Malaysian Govt/TSB
3. Biodiesel screening [PhD] EPSRC
3. Catalysis: 1. Heterogeneous, Biodiesel [PhD] EPSRC
2. Vegetable oil cracking [PhD] Indonesian Govt.
3. Catalytic cracking of algae [PhD] Nigerian Govt.
+ various other biofuel/biorefining projects (Intensification of phytoremediation about to start 2013)
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Case Study 1: A Saponification reaction
in an Oscillatory Baffled Reactor
Achieves plug flow
by tanks in series
rather than
turbulence
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OBR characteristics
Long residence times in a compact
reactor, whilst maintaining plug flow
and good two phase mixing.
Niche:
BATCH CONTINUOUS
For “long” processes
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The Reaction
Hydrolysis of a naturally occurring mixture of
alkyl and steryl stearates, using
concentrated sodium hydroxide in an
ethanol and water solvent.
75 m3 Batch Reactor [50 m3 fill]
115 oC
2h "reaction time” in a 24h batch cycle
Molar ratio ~ 0.9
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Incentives for Change
1. SAFETY 2. Product quality
3. Energy savings
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Experiments Conducted
Temperature fixed at 115 oC
Molar ratios in the range 0.6 - 1.05
Residence times in the range 8 - 25 minutes
TARGET PRODUCT
Desired product, sterol A > 23 %
Undesired product, sterol B < 10 %
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Can it be done ?
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Effect of Temperature (modelling)
(+ the modelling wasvalidated by experiment!)
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Operating Windows
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Monitoring: FTIR ATR Cell
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SUMMARY: OBR Saponification
The OBR could be used to perform the reaction:
..at lower temperature (safer, reduced energy)
..with improved product quality
..more consistently
..in 1/10th the reaction time (inherent kinetics)
..in a reactor 1/100th the volume
The product can be monitored online
Operation is flexible (wide operating window)
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Was the reactor built?
No!
“Champion” made redundant!
No "risk takers“ remaining
Lack of understanding (company dominated
by chemists...)
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Recent Directions for OBRS @
Newcastle
1. Mesoscale OBRs (<6mm diameter)
2. Bioreactions
3. Crystallization
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“Meso OBRs”: What are they?
(a) Integral baffles
(c) Central baffles
(b) Helical baffles
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Meso OBR: Platform
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Meso OBRs: What are they for?
Features:
Low flow rate
Can suspend solids
Controllable mixing of L-L systems
Uniform shear
Plug flow
Residence times of the order of hours in
reactor a few metres in length
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MesoOBR Application:
Imine synthesis
• Fundamental role in several applications
biological process
polymeric substance synthesis
dynamic combinatorial chemistry
• Reaction can be followed by IR in situ
• Entirely liquid phase
Benzaldehyde N-butylamine
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MesoOBRs: “Dynamic Screening”
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MesoOBRs: “Dynamic Screening” Validation
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MesoOBRs: Multivariate Screening, or
“Dynamic Design of Experiments”
0.00
0.02
0.04
0.06
0.08
0.10
0.12
0
50
100
150
200
250
3000.8
1.01.2
1.41.6
1.82.0
2.2
concentr
ation (
mol dm
-3)
time (s)
ratio
Benzaldehyde reduction profile for different ratio and screening method
dynamic (1 to 2)
steady state (1:1)
steady state (1:1.5)
steady state (1:2)
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MesoOBR: Biodiesel
Biodiesel with heterogeneous catalysts
as a familiar example of L-L-S reactions
to trial
Benchmarking with homogeneous
catalysts led to some interesting
results...
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Effects of Residence Time, Catalysts and
their Concentrations on the FAME Content
Effects of residence time on FAME content at different catalysts concentrations
for RSO transesterification at 6:1 methanol/RSO molar ratio, Reo = 160, T = 60˚C.
70
80
90
100
0 5 10 15 20 25
% A
vera
ge F
AM
E a
t ste
ad
y s
tate
Residence time (mins)
0.75 wt% NaOH 1.0 wt% NaOH 1.0 wt% KOH
1.0 wt% NaOCH3 1.5 wt% KOH 1.5 wt% NaOCH3
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Effects of Reaction Time on the FAME
Content (Numerical Model)
Effects of reaction time on FAME content at different catalysts concentrations for KOH
catalysed transesterification at 6:1 methanol/RSO molar ratio, 60˚C and 1% (w/w) water
based the RSO (** 5 wt% water).
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MesoOBR: Biodiesel
1.Reaction times of only 2 minutes required
2. ..but conversion drops thereafter
3. .. so control of conditions has to be tight for this
to be realised/observed
4.Modelling clearly shows that this is due to the
relative rates of the competing transesterification
(biodiesel-forming) and saponification reactions,
and this has been validated by experiment.
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OBBs: Oscillatory Baffled Bioreactors
Batch Oscillatory Baffled
Bioreactor: BOBB
Self-contained
Autoclavable
Used for ABE fermentation
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O.F. Mixing Enhances Cell Growth
0.02 0.05 0.05 0.06 0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0 470 938 1870
Glu
cose
co
nsu
mp
tio
n r
ate
(g
/L.h
)
Spe
cifi
c gr
ow
th r
ate
(1
/h)
Reo
Specific growth rate, μ Glucose consumption rate
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ABE productivity in BOBB and STR
0.16
0.21 0.22
0.13
0.16
0.19 0.2
0
0.05
0.1
0.15
0.2
0.25
0.00 0.02 0.10 0.83
Solv
ent
pro
du
ctiv
ity
(g/L
/h)
Power density (W/m3)
BOBB
STR
Objectives PI Bioreactors ABE Findings Conclusion
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ABE production per unit energy
Objectives PI Bioreactors ABE Findings Conclusion
13
2.1
0.14
9.9
1.8
0.24 0
2
4
6
8
10
12
14
0.02 0.10 0.83
AB
E p
rod
uct
ivit
y p
er u
nit
p
ow
er (
g A
BE/
kW.h
)
Power density (W/m3)
BOBB
STR
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OBRs: Current State of
Commercialisation
1. Various under development with “NiTech”
(Glasgow, UK)
2004 – 2006: Industrial unit, James
Robinsons’, UK
2. Various in operation “behind closed doors”
3. First mesoreactor system sold, 2012
4. Pilot-scale facilities available at Centre for
Process Innovation (CPI), Teesside, UK
(mostly for biological processes)
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Acknowledgments
Dr Anh Phan
Nasratun Masngut
Fatimah Mohd Rasdi
Valentine Eze