ILS Presentation - Integrated Lab Solutions

Providing Chemical R&D
Solutions
Company Presentation
NON-CONFIDENTIAL
www.integratedlabsolutions.com
ILS-Integrated Lab Solutions
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•
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Berlin Based
Designs & Builds custom R&D Testing Systems
Offers Chemical R&D Testing
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Heterogeneous Catalysts
Homogeneous Catalsts
Corrosion/Erosion
Combustion
Sequestration testing
Hydrate Testing
2
People: Our Most Important Asset
•
26 Employees
- 6 PhD Chemical Engineers
- 1 M.S. Chemist
- 1 M.S. Chemical Engineer
- 6 M.S. Mech. Engineers
3
Worldwide Supplier
Over 100 units made since 2004!
USA
-Houston
-San Francisco
-Little Rock
Germany
Belgium
Netherlands
France
Finland
Switzerland
UK
Saudi
Arabia
UL & ASMEcompliant units!
S. Africa
4
Well-Established Client Base
5
ILS Focus Change
ILS recognizes clear market opportunity
-
Expand production in 2013 to meet rapidly
growing demand
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Set-up contract R&D Laboratory in 2013 to
extend from enabling tools to contract R&D
R&D Enabling
HARDWARE &
SOFTWARE
Contract R&D
SERVICES
6
Project Execution with ILS
Enabling-Tools
Typical Project Execution
Pre-Engineering
-P&ID‘s
-Design Note
-HAZOP
-Relief Calculations
-Component List
-Electrical Drawings
1 Month
SAT at Client
Detail-Engineering &
Component Delivery
-3D CAD (Inventor)
-GUI
-Programming Typicals
2-3 Months
Build & Test
-FAT
2-3 Months
1-2 Months
8
Project De-Risking
Project De-Risking
Alternative Project Execution Options
OPTION 1: Proof-of-concept BEFORE
commitment to full-scale unit
• Short-Term realization (1-3 months)
• Minimal Investment (50-100k€)
OPTION 2: Extend feasibility to provide data during build of full-scale
unit!
1-3 Months
1 Month
2-3 Months
2-3 Months
PreEngineer
DetailEngineer
Build
1-2 Months
OPTION 3: Chemical Commisioning BEFORE
Delivery
9
Feasibility Study
Selective Olefin Hydrogenation
Example 1: Feasibility Study
Selective Olefin Hydrogenation
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Designed unique lowtemperature reactor design
Built & commissioned 4parallel unit in 3 months
Configured & calibrated GC
parallel to build
1-month feasibility executed
Client opted for additional
contract R&D on unit after
successful feasibility
- Data generated during
production of 16-parallel
unit!
4-Parallel Feasibility Unit
Unique, Low-T
Reactor
Design
11
Example 2: Feasibility Study
Continuous Zeolite Membrane Synthesis
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•
•
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Unit built in 2-months
3 months of contract R&D
performed on unit
Extensive testing with
zeolite slurries
EDX and permeability
experiments performed
Successful Feasibility lead to
construction of full-scale 8parallel unit.
Full-Scale 8-Parallel Unit
IR Imaging to identify „hot“
and „cold“ spots
12
Chemical Commissioning
Monolith deNOx Testing Unit
EXAMPLE-Chemical Commissioning
-Parallel deNOx Testing
Specifications:
•
3 quartz reactors operated in
parallel
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850°C
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Improved heating/cooling rates
•
ILS provided complete Analytics
• iAG MKS FTIR Analyzer
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Rich/Lean Switching on all reactors
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Improved Sample Holder Design
14
EXAMPLE-Chemical Commissioning
Rich/Lean Switching
2000
1000
0
0
Reproducible with true
2 form
4
delta
[bar]
CO
NO
NH310
6
8
6
Common
Transient 1
8Transient 210
6
PIC510.WSP
PIC510.PV
PIC430.PV
8
10
50
3
[dm /min]
[ppm]
Step verification test Reactor 200°C
0
0
2
1.5
1
0
Total Flow=Constant
2
Upstream
2
Minimal Impact on
Pressure
Downstream
4
4
Time [min]
15
Example Units
-Hydroprocessing
-GTL
-Gas/Vapor-Phase examples
8-Parallel SRGO-VGO HDS-HDN Units
Specifications:
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8 Individual Reactors
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1-10g Catalyst
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Online stripping
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Takes up to 10 samples
automatically
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Individual product-gas
flow measurement
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Max 300 bar
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Map T=600°C (3 zones)
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Heated Feed & Product
Vessels for heavy feeds
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Weighed feed & Product
vessels
Compressor Station:
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Electrical compressor
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Up to 300 Bars
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Fully Automated
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Fully Integrated with
unit
17
Bitumen Hydrotreating
-Trickle Flow/Process Optimizer
Specifications:
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EXTRUDATES
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4 reactors
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3-Zone master/slave heating
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300 bar, 600°C
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Integrated Hydrogen Compressor
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Automated sample collection and weighing
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Operates at VERY low LHSV (0.05 to 0.1hr-1)
•
Operates with highly-viscous feeds (all feed vessels and pumps heated to 200°C)
•
Online GC
18
Bitumen Hydrotreating
-Semi Batch/Mo-& Fe-Sulfide Additives
Specifications:
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4 Parallel
Hydrotreating
reactors
•
Max T=550°C
•
Max P=250 Bar
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Gas uptake
measurement
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Hot and cold G/L
separators
•
Fully Automated
19
Cellulose/Hemicellulose Hydrotreater
Bottom-Up Flow
Specifications:
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4 Reactors
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150 Bar
•
Hastalloy for work with
corrosive solvents
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300°C
•
2-Phase backpressure
control
20
16-Parallel Trickle-Flow Hydrotreater
Multipurpose Unit
Specifications
• 16-Reactors
• 4-Temperatures
• 4-Pressure zones
• 4-liquid LHSV’s/16 reactors
• 4-GHSV’s
• True plug flow even at low LHSV
• 30cm isothermal zone (+/-1°C at
500°C)
• Disposable quartz/StainlessSteel reactors
• Quick, manual closure opens 16
reactors in ca. 20 seconds!!!
• Max T=500°C
• Max P=200 Bars
• Gas & Liquid Dosing
• 3 integrated on-line GC’s
• 16-parallel liquid sampler
• Fully Automated
21
2-Phase Backpressure Control
• No g/l separators needed!
• Rapid de-gassing of saturated gases =
better on-line analysis
• Works with viscous Bitumen and VGO
Ultra Wide Flow Range Performance
EB1LF Air Trials
Air Flow, SCFM
4E-6
4E-5
10000
4E-4
4E-3
4E-2
4E-1
4E+0
Various Set Points: .04, 0.2, 1, 6, 30, 300 and 1000psig
1000
60,000
6,000
100
600
10
60
1
6
0.1
1
Inlet Pressure, kpag
Inlet Pressure, psig
4E+1
HUGE
turndown ratio!
0.01
0.1
1
10
100
1000
Air Flow, ml/min
10000
100000
1000000
22
Biodiesel Pilot Plant
Specifications:
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Hydroprocessing
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2 Trickle Flow Reactors
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2000mm Long
•
7-Zone heating
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Parallel or recycle operation
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600°C
•
300 Bar
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Complete Distillate Workup
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Vacuum Distillation
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Fully Automated
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Package Unit
23
Example Units
-GTL
Simultaneous Production of 8 GTL Units
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8 x Fixed-Bed Reactors
1-3g Catalyst
650°C
100 Bar
Peltier-cooled g/l separator for
gas/liquid separation
Liquid Feed Vaporizer
HPLC with weighed liquid feed
vessels
Liquid Sampling
Ability to create mixed-gas
feeds
Custom high-turndown
backpressure control
Online GC
Fully Automated with Trending
Fully-enclosed & ventilated
ITEM Profile enclosure
25
4-Parallel Fischer-Tropsch Unit
INDEPENDENT Master/Slave Control Keeps FT Exotherms under
control! (note oven can be 20-30°C cooler than reactor inner
temperature!!!!)
Specifications:
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Fixed bed
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2 to 7mm i.d. reactors
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550°C max T
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In-Situ Reduction
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CO/H2 gas alarms
•
Online GC
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COMPLETELY independent reactors
(T, P, gas flows)
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Screen at similar conversions to
prevent diffusion limitations from
influencing selectivity profiles!
26
32-Parallel Fischer Tropsch Fixed-Bed Unit with finger-tight
reactor design
Specifications:
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32 reactors
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16-Reactors for long-time runs (1 month +)
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16-Reactors for short time runs (2 days to 4 weeks)
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100 bar, 500°C
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2 stage wax/water/gas separation
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2 x On-line GC‘s
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Abilits to co-feed olefins and water
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Finger-tight reactor closure
27
16-Parallel Methanol Synthesis
INDEPENDENT HEATING!
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16 Reactors
INDEPENDENT Heating (max 550°C)
Common P (max 100 Bar)
Common gas/vapor feed
2 x online Micro-GC‘s
Note excellent reproducibility!
Independent heating makes rapid
kinetic testing possible! (4
temperatures used during kinetictesting pahse)
From PhD Thesis, T. Henkel, TU
Munich,2011
28
Compact Fischer-Tropsch CSTR System
Slurry!
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300°C
100 bar
Carbonyl Trap
Efficient Slurries separation
Automatic liquid-level control in CSTR
Hot G/L Separator for wax/steam separation
Cold G/L Separator for Water/gas separation
On-Line GC
Fully-Automated
29
4-Parallel, CSTR Slurry-Phase Fischer-Tropsch
Process Optimization Unit
Specifications:
•
4 x 3 Liter Reactors
•
Simulates complex
syngas feeds (10
components)
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Slurries separation
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Olefins addition
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Water addition
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Wax/Water Separation
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Water/Gas Separation
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Degassed components
re-combined &
measured by GC
•
Online GC
30
FT-Co/Al2O3 Reduction Reactor
Fluidized Bed
Specifications:
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Fluidized Bed
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ATEX Zone 1 Compliant
(nitrogen overpressure)
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Reactor is completely
enclosed in N2-cabinet
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External water cooling of
high-T oven
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500°C max T
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4-Zone Heater
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50Barg max P
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Conventient „sled“ system
for opening & closing
reactor
•
Reduce up to 50g of
catalyst
ATEX
Protection
Oven
CLOSED
Split-shell
heater OPEN
ATEX
Protection
Oven OPEN
31
Gas-Phase Applications
-Aromatic conversions
-Partial Oxidations
-Pygas Synthesis & Ethylene
Oligomerization
-Methanol Synthesis/Steam Reforming
-Partial Oxidations
16-Parallel Aromatics Conversion Reactor
Specifications
• 16-Reactors
• 4-Temperatures
• True plug flow
• 20cm isothermal zone
• Independent pressure control
• Exchangeable quartz/Stainless-Steel
reactors
• Simple, disposable reactors
• Quick, pneumatic closure opens 16
reactors in ca. 20 seconds!!!
• Max T=500°C
• Max P=100 Bars
• Gas & Liquid Dosing
• Custom design for extra wide pressure
and GHSV range
• 2 integrated on-line GC’s
• Fully Automated
33
Combinatorial Chemistry & High Throughput Screening
2012, Vol. 15, No. 2
Acrylic Acid Synthesis Results
10-Parallel Reactor
INDEPENDENT Heating!
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•
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500°C
50 barg
Downstream N2 pure prevents tar formation
downstream and blockage.
Disposable Reactors
Pressure control in EACH reactor
4 Temperature Zones
Common Gas & Vapor to all reactors
Can dose up to 90% water vapor!
Independent heating makes
rapid kinetic testing
possible!
34
Acrylic Acid Synthesis-Excellent Reproducibility
Despite Product Polarity and Self-Polymerization
C3
CO-x
Acrylic Acid Carbon
conversion Selectivity Selectivity Balance
6/3/40/51 5000h-1 350degC
d=4mm
26%
70%
20%
96%
d=2mm
35%
25%
70%
95%
35,0%
Strong Sensitivity to
Backmixing!
30,0%
25,0%
X propane
20,0%
S acrylic
acid
15,0%
10,0%
5,0%
0,0%
35
4-Parallel Process-Optimization Reactor
Py-Gas Hydrogenation
Olefins-to-Gasoline
Specifications:
• 4 x Fixed beds
• ½“ OD reactors
• 600°C max T
• Gas & Liquids Feeding
• In-Situ Reduction
• Flammable/H2 gas alarms
• Online GC
• COMPLETELY independent
reactors (T, P, gas flows)
36
Temkin Reactor
Mimics hydrodynamic conditions of a full-scale fixed-bed reactor
= Better Scale-up!!!
Ideal for egg shell-type
catalysts (no crushing required)
37
Vinyl Acetate Monomer Synthesis Testing on Real
Impregnated, Shaped Catalysts
Propane & C3 Oxidation in a
simulated Fixed-bed Temkin
Reactor
Specifications:
•
Corrosion resistant
materials, PEEK®,
Hastelloy®C276
•
20 bar, 500°C
•
Online GC and IR
•
7 fold
•
Egg-shell catalyst testing
Taken from: G. Mestl Combinatorial
Chemistry & High Throughput
Screening, 2012, 15, 000-000
38
New Generation Süd Chemie VAM Catalysts
Developed with Temkin Technology
Taken from: G. Mestl Combinatorial
Chemistry & High Throughput
Screening, 2012, 15, 000-000
39
Unique Internal-Recycle Reactor
Licensing Agreement with Prof. Wasserscheid-University of Erlangen
Specifications:
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500°C
•
HC276 or 316SS
•
100 Bar
•
15.000RPM!!!
•
Operates at LOW and
HIGH pressures!!!
•
Powders or extrudates
•
Gradient-free operation
40
Unique Internal-Recycle Reactor
Licensing Agreement with Prof. Wasserscheit-University of Erlangen
Excellent correllation between:
-Bo calculated from RTD analysis
-1-Butene Conversion (at 10 bar)
Powerful tool for:
-Kinetic Testing
-Simulating fluidized-bed
conditions
41
High-Shear Reactor for
Erosion/Corrosion Testing
Specifications:
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500°C
•
200 Bar
•
High-Shear FCC Bottoms
Erosion Testing
•
4-Samples in Parallel
•
Integrated low-shear
reactor
•
Erosion measured by
weight loss.
•
Slurry recycled with
minimum residence time
in hot zone (minimizes
cracking)
42
Content:
• Polyolefins Solutions
40 Parallel Polyolefins Catalyst Testing
For air/moisture-sensitive chemistry!
Specifications:
•
40 Reactors
•
Manual control, multiple
temperature and pressure
zones
•
100 bar, 200°C
•
Extremely robust
•
Easy to learn
•
low maintenance
44
WORKING WITH AIR & MOISTURE
SENSITIVE CATALYSTS
dP=
0
Pressure
equilibration
Needle
Rubber
Septum
Pressure
Vessel
Glass
Liner
Magnetic
Stirrer
KFUPM
45
20-Parallel Polyolefins Unit
KAUST-University
Uni Lyon-R. Birrer/Boisson
20 Autoclaves
Specifications:
•
200°C, 100 bar
•
Heated in blocks of 10
•
Pure Batch Operation
•
No Cleaning required
46
Investigation of a conventional heterogeneous ZieglerNatta catalysts
Test
Results
Activity (usual conditions)
OK
Reproducibility
OK
Polymer morphology
OK
Investigation of a metallocene precursor in combination
with methylaluminoxane
A series of experiments with increasing concentration of catalyst
were performed
All tests were successful including those performed
at low concentration of Zr (3 mM)
47
Process-Optimization Catalyst Testing
Ethylene Oligomerization
4 Independent Autoclaves
Specifications:
•
300°C, 100-200 bar
•
Independent heating and
cooling for exotherm control
•
Fully automated with recipe
control
•
Continuous gas flow
•
Optional liquid sampling
during reaction
48
4-Parallel Batch Process Optimizer
Integrated Cat-Prep Robot in Glovebox
Cat-prep robot
in glovebox
Inert-glovebox
atmosphere
Easy Reactor Removal &
Cleaning (pneumatically raised &
lowered)
49
Spherical Reactor for Gas-Phase Polyolefins
Synthesis
Specifications:
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8 Liter
•
Steam/water heating-cooling
•
Ideal polymer morphology
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Kinetic-Quality Data
•
Custom Stirrer Design
•
ATEX-Explosion Proof
•
TüV approved
50
Content:
• Polyamide Solutions
http://theses.insa-lyon.fr/publication/2013ISAL0019/these.pdf
Polyamide (PA66, PA11) Synthesis Reactor
(Melt-condensation polymerization)
Specifications:
•
1 Liter
•
60 bar
•
360°C (also inside Mag drive)
•
Sapphire Glas window
•
Very precise Temperature (+/- 0.5°C)
and Pressure control (+/-0.05bar)
over the whole range
•
Liquid dosing with HPLC pump
•
Torque sensor
•
Special Bottom drain valve
•
Water collection system with
condenser and balance
52
http://theses.insa-lyon.fr/publication/2013ISAL0019/these.pdf
Results
Condensation of a mixture of
isophthalic
and FDCA acids with hexamethylene
diamine
53
Content:
• Polystyrene Solutions
Polystyrene Pilot Plant with Devolatizer
Ethylbenzene and Styrene Monomer Storage (ATEX)
•
•
•
•
•
20 Liter Pilot Scale
Polystyrene Synthesis
Including inline devolatizer
Fully Automated
All piping and vessels double-jacketed to
280°C to prevent cold-spot formation
-Polystyrene Pilot
-Monomer Devolatizer
55
200Nm drive with Torque sensor
20L reactor (dj) with double
helix stirrer
Emergency injection vessel
(dj)
Static mixer and heat
exchanger (dj)
18L Devolatizer (dj)
with window and light
source
Gear pump (dj) (Maag)
Bottom drain valve (dj)
(Schuf)
56
High-Throughput Hydrogenations
Parallel Assymetric Hydrogenation Unit
•
•
•
•
•
•
94, 48, 20 and 10 Parallel
units have been made
Max T=300°C
Max P=200 Bars
Common Gas atmosphere
Minimal crosstalk
Excellent isothermicity!
58
High-Throughput Supercritical CO2
Testing
High-Throughput CO2 Testing Unit
4-Reactors in ONE Unit
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24-Parallel Slurry Testing
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10-Parallel Zeolite Testing
•
Single Fixed-Bed for lifetime
studies
•
Visualization Reactor
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Max 200 bar
•
Max 200°C
•
Fully-Automated
60
High-Throughput CO2 Testing Unit
Ionic Liquid Catalysts for Chemical Fixation of CO2 to
produce cyclic carbonates
Aprile, Giacolone, et al. ChemSusChem 2011, 4, 1830-1837
61
High-Throughput Zeolite
Synthesis in Supercritical CO2
Titanium-based Photocatalysis Synthesis
Jammaer, Aprile, et al. ChemSusChem 0000,00, 1-8
62
Separations Technologies
High-Throughput Zeolite Adsorbent
Testing
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20 Fixed-Bed Reactors
Max P=200 bars
Max T = 500°C
Independent Gas dosing
Rapid SERIES adsorbent
Testing
On-line LIQUID GC (for
online analysis)
On-Line Liquid Sampler (for
offline analysis)
64
Breakthrough curves
show selective
adsorption of toluene
Delta Pulse shape proves
true plug flow (essential
for kinetic studies!)
65
Continuous Zeolite Membrane Synthesis
SAPO Membranes for Selective Gas Separation
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•
•
•
8 Continous-Flow
Membrane Synthesis
Reactors
Slurries Compatible
pumps
Use of large ovens for
heating & easy access
Fully Automated
66
HF/Water Equilibrium Testing Unit
Corrosion-Resistant Calorimeter
•
•
•
•
•
•
Batch Calorimeter
Automatically Detects boiling
points
Used for determining HFWater vapor/liquid equilibria
Teflon-lined reactor for
corrosion resistence
Hastalloy & Monel
components for corrosionresistent pressurecomponents
Fully-automated, highpressure water and HFsampling
67
Automotive Testing Units
Diesel Catalyst Test Unit
Testing of Diesel particle Filters
Specifications:
•
2 Steady state quartz
reactors (Tmax=1000°C)
for Diesel Particle Filters
•
1 High dynamic oven
(Tmax=850°C; 50°C/min)
for DeNOx storage cats
•
36 MFCs, 4 evaporators
•
Integrated FTIR, FID,
MS, Lambda sensors
•
Applicable for monoliths
and other structures
69
Ultra-Compact Diesel deNOx
Testing of Diesel particle Filters
Monolith Testing Unit
Specifications:
•
1 Steady-state quartz
reactors (Tmax=1000°C)
for Diesel Particle Filters
•
10 MFCs, 2 evaporators
•
Integrated FTIR, FID,
MS, Lambda sensors
•
Applicable for monoliths
and other structures
70
Requirements for testing DeNOx catalysts:
•
•
•
•
Pulsation free
Plug flow
Stable gas flows
Rich/Lean switching with 1-3Hz
High dynamic oven
71
deNOx /DOC /ASC flexible Test Unit
Testing of SCR, deNOx, DPF:
•
1 High dynamic oven
(Tmax=1000°C;
50°C/min)
•
20 MFCs with flexible
valve routing for wide
operation range
•
Automatic MFC
calibration
•
Dynamic concentration,
pressure, flow changes
•
Integrated FTIR, FID,
MS,
•
Applicable for monoliths
and other structures
72
Rapid Temperature Ramping
Excellent Isothermicity
Temperature Steps 45 dm3/min
600
Temp. [C]
500
400
300
200
100
0
0
50
100
Time [min]
TIC500.PV
TIC501.WSP
TIC501.PV
TIC502.WSP
TIC502.PV
TIC503.PV
TE 504.PV
150
200
73
Excellent Isothermicity
Temperature Profile Reactor 1
1000
900
Axial Temperature [°C]
800
700
Zone 1 and 2 at 500°C, with 20 NL/min
N2 flow; centered inlet
600
500
Zone 1 and 2 at 500°C, with 100 NL/min
N2 flow; centered inlet
400
Zone 1 and 2 at 850°C, with 20 NL/min
N2 flow; centered inlet
300
Zone 1 and 2 at 850°C, with 100 NL/min
N2 flow; centered inlet
200
100
0
0
10
20
30
40
Distance from Frit [cm]
74
Rich/Lean Switching
2000
1000
0
0
2
4
[bar]
CO
NO
NH310
6
8
6
Common
Transient 1
8Transient 210
6
PIC510.WSP
PIC510.PV
PIC430.PV
8
10
50
3
[dm /min]
[ppm]
Step verification test Reactor 200°C
0
0
2
1.5
1
0
2
2
4
4
Time [min]
75
Minimal Ammonia Holdup
40
20
0
0
[bar]
[dm /min]
2000
1000
0
0
3
[ppm]
NH3 holdup test Reactor 200°C
3
2
1
0
2
2
2
4
4
4
Time [min]
CO
NO
NH310
6
8
6
Common
Transient 1
8Transient 210
6
PIC510.WSP
PIC510.PV
8
10
PIC430.PV
76
Diesel Particle Filter DeNOx Test Unit
Testing of complete particle
Filters
Specifications:
•
3 quartz reactors
•
850°C
•
Ultra-Fast IR heating zone
•
300l/min gas flow
•
Integrated FTIR
•
Applicable for monoliths
and other structures
IR Oven
77
Fuel-Combustion Testing Units
Turbulent Combustion Reactor
•
•
•
•
•
•
•
•
550°C
100 Bar
Fuel Injection
Glow coil & tunable spark
4 Visualization Windows
300kHz Pressure Measurement
300kHz Flame Ionization Detector
Schlieren imaging with 50kHz
Laminar Combustion Sphere
(under construction)
78
Upstream R&D Testing Units
24-Parallel Hydrate Inhibitor Unit
•
•
•
•
•
Screen 24 thermodynamic or kinetic
hydrate inhibitors in parallel
Max 200 bars
NACE compatible (for use with high
Chlorine brines and H2S)
Complete immersion of reactors AND
piping & valves for perfect isothermicity
No-Cleaning required due glass-liner use
80
6-Parallel Raman-In Situ CO2
Sequestration Unit
•
•
CO2 Sequestration
- 6-Parallel Unit
- In-situ Raman
Brine/Rock/CO2 Kinetic Testing
81
Contact Us!
ILS-Integrated Lab Solutions GmbH
Max-Planck-Strasse 3
12489 Berlin, Germany
+4930263966910
www.integratedlabsolutions.com

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