ynamische sorptionsuntersuchungen am system … · solvent/voc (depends on t and p) → be sure...
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J. Möllmer
DYNAMISCHE SORPTIONSUNTERSUCHUNGEN
AM SYSTEM VOC/AKTIVKOHLE
Institut für Nichtklassische Chemie Leipzig e.V.
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Outline
-2-
• Effects influencing breakthrough curve measurements
→ Dosage of organics
→ Requirements
→ Limitations
• Example I (VOC separation from
biomass plant)
• Example II (VOC/humidity on AC)
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
-3-
VOC – Volatile Organic Compounds
Contamination leads to massive health issues like
Cancer, Liver and kidney damage
Central nervous system damage
Vaporizable, carbon-containing compounds
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Overview – examples for VOC separation
-4-
Sorption with activated carbon
Thermal or catalytic
decomposition
→ Breakthrough Testing
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Overview – Principle of Breakthrough Measurement
-5-
Dosage system
Thermostated unit
Reactor/Adsorber
Detector
Mass flow controller bubbler
Glass or metal
version
FID, MS, IR, electrochemical,
others
Off-gas treatment (optional)
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Dosage system – Example I
-6-
Providing a saturated inert gas flow by
- Bubbling with inert gas through one bubbler
Pro Contra
- No heater needed - Only for pure organics
- Easy handling - c0 depends on fill level
adsorber
decrease in c0
often
no constant dwell time
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Dosage system – Example II
-7-
Providing a saturated inert gas flow by
- Bubbling with inert gas through two bubbler
Pro Contra
- No heater needed - Only for pure organics
- Nearly constant c0 - More complex handling
adsorber
constant c0
nearly
constant dwell time
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Dosage system – Example III
-8-
Providing a saturated inert gas flow by
- Heater/vaporizer – direct injection
Pro Contra
- Miscible liquid mixtures possible - Heater is needed
- Direct control of c0 - Complex equipment
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Dosage system – limitations
-9-
→ Larger concentration is limited due to the csat of the used
solvent/VOC (depends on T and p)
→ be sure that no condensation can occur (heating up tubes)
→ Low concentration is limited due to the csat of the used
solvent/VOC (dilution; lower T possible)
→ normally dilution down to 1:500 works (dilution depends
also on overall flow)
→ Dilution below 1:500 – use premixed testing gases !!!
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Reactor/Adsorber
-10-
Reactor differs in size and geometry
→ dbed : dParticle > 10:1
→ hbed : dbed > 3:1
To do:
- Check bed parameters depending on particle size
- Check bed length and velocity for pressure drop
H.W. Kajszika, Adsorptive Abluftreinigung und Lösemittelrückgewinnung durch Inertgasregenerierung, Utz Verlag, 1998.
dbed = 40 mm
Early breakthrough on wall
→ curve flattens
Minimization of
Bypass flow
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Reactor/Adsorber
-11-
Reactor differs in size and geometry
→ dbed : dParticle > 10:1
→ hbed : dbed > 3:1
To do:
- Check bed parameters depending on particle size
- Check bed length and velocity for pressure drop
H.W. Kajszika, Adsorptive Abluftreinigung und Lösemittelrückgewinnung durch Inertgasregenerierung, Utz Verlag, 1998.
dbed = 40 mm
Early breakthrough on wall
→ curve flattens
Minimization of
Bypass flow Shift
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Detector
-12-
Depends on analytical question
• Number of compounds
• Concentration range (detection limit depends on scope,
but should be at least 100-1000 times lower as c0)
• Check time resolution for online GC systems or ECD
• Coupled systems possible → be sure if the overall flow is
large enough for all analytical devices (e.g. aspirated
IR or µGC)
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Dead time correction
-13-
• Dead time or volume – time is needed for flowing the bed up
to the detection unit
fast process
• Avoid interaction between VOC and tubes/fitting/sealing
• Avoid back mixing in the whole system
Input function –
ideal flow tube
non-PTFE type tube
as transfer-line to FID
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
-14-
Summary I
→ Breakthrough measurements can be a complex scenario
→ Modular concept ensure high flexibility
→ Check process conditions and select equipment, but
Down-scaling your process, be careful
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Example I - Biomass gasification
-15-
• Gasification of lignocellulosic biomass, mostly:
• Biomass → Gasification → Purification → Turbine/
Power plant
• Gasification agents: Air, O2, Steam, (CO2)
• Product gas contains: H2 35-45%, CO2 20-25%,
CO 19-25%, CH4 9-11%, CxH2x+y 3-4%, impurities
like benzene, toluene, styrene, …
wood chips
cereal or maize straw
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test
-16-
Characterization of activated carbon
Isotherms Breaktrough experiments
Static method Dynamic experiment (fixed bed)
Hexane
Cyclohexane
Benzene
Toluene
reactor pump
to GC
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Experimental section: Breakthrough Curves
-17-
DynaSorb BT:
→ Dynamic method
→ Fully automated
→ Different adsorber sizes available
→ Temperature measurement inside the
adsorber bed
→ Data collecting and data evaluation
tools (with simulation according LDF-
approach)
DynaSorb BT
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test: isotherms
-18-
toluene benzene cyclohexane
hexane
relevant concentration range
• Affinity: toluene > benzene >
cyclohexane > hexane
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test: breakthrough curves
-19-
• Breakthrough of pure vapors benzene and toluene at 35 °C
Variation of c Variation of velocity
• Lower concentration leads to larger breakthrough time
• Higher velocity leads to decrease in breakthrough time
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test: breakthrough curves
-20-
• Determination of kLDF from breakthrough experiments at 35 °C
pure
components
(constant
velocity)
toluene benzene cyclohexane hexane
~ 1000 ppm
kLDF / 10-4 s-1 1.75 1.73 1.94 4.33
~ 4500 ppm
kLDF / 10-4 s-1 4.60 4.21 4.27 8.64
~ 9000 ppm
kLDF / 10-4 s-1 6.88 7.57 6.72 10.67
Lorimier et
al. 2005 3.2 – 5.8
C. Lorimier, A. Subrenat, L. LeCoq, P. Le Chloirec, Environ. Technol. 26 (2005), 1217-1230.
• kLDF depends on molecular size:
hexane > benzene > toluene/cyclohexane
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test: breakthrough curves
-21-
• Breakthrough of mixed vapors benzene/toluene at 35 °C
• Benzene is displaced by toluene
• Slope of toluene breakthrough flattens
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Adsorptive Purification – Lab test: breakthrough curves
-22-
• Breakthrough of mixed vapors benzene/hexane at 35 °C
• Benzene is displaced by hexane at low hexane concentration
• Traceable concentration effects
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
-23-
Example II – Effect of humidity to sorption of VOC
Important case of application: Effects of humidity
• Waste air/exhaust air cleaning
→ Humidity depends on
conditions at location
http://www.silica.berlin/de/
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Example II – VOC vs. H2O sorption on AC
-24-
• Completely different sorption behaviour due to difference
in physico-chemical properties
IUPAC Technical Report, Pure Appl. Chem. 2015; 87(9-10), 1051-1069
VOC
H2O
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Breakthrough curve – H2O
-25-
H2O breakthrough at different concentrations
→ H2O breakthrough below inflection point of isotherm shows
typical shape, at higher concentration a stepwise curve is
observed due to capillary condensation
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Breakthrough curve – H2O
-26-
Below 45% RH Above 45% RH
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Breakthrough curve – H2O (low affinity towards AC?)
-27-
→ Strong heat detection during first adsorption due to large
interaction of H2O with ash content of carbon
→ Second heat peak is provided by heat of vaporization
Type V isotherm is coupled with a low affinity?
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Breakthrough curve – Benzene
-28-
Benzene capacity is influenced by humidity
→ Benzene breakthrough flattens for low H2O concentrations
→ Benzene capacity decreases with increasing H2O content
Capacity decreases
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Breakthrough curve – effect of pre-wetting
-29-
Benzene capacity is influenced by pre-wetting of the AC in
dynamic (breakthrough) experiment
→ Capacity of benzene decreases after pre-wetting the AC
→ Long equilibration time for H2O sorption (due to capillary
condensation) leads to an unachievable equilibrium case
Capacity decreases
Kinetics play a major role
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Summary II
-30-
• Breakthrough test ideal for Process Down-Scaling
→ Check general experimental conditions
• Studying sorption under real conditions
→ Kinetics
→ Thermodynamics
→ Detection of heat effects
→ Competitive sorption (complex mixtures possible)
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
Acknowledgement
-31-
INC Team
Many thanks for your attention!
http://research.uni-leipzig.de/inc http://www.dynamicsorption.com/
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Leipziger Symposium 2017
Leipzig, 30.05.2017
Institut für Nichtklassische Chemie e.V.
http://research.uni-leipzig.de/inc/
-32-
References
https://www.helsa.com/helsa-functional-coating/helsa-sorbexx/produkte/helsasorbexx-gs/
http://www.adfis.de/index.php/aktivkohle-fur-aktivkohlefilter/
http://www.dge-wittenberg.de/
http://www.silica.berlin/de/
https://www.slideshare.net/SaifulIslam156/adsorption-process-for-voc-volatile-organic-compounds-copy
https://www.vdi.de/technik/artikel/abgasreinigung-verfahren-der-katalytischen-abgasreinigung-grundlagen-3/
http://www.autobild.de/artikel/katalysator-aufbau-funktion-und-schaeden-8533435.html
http://ecolink.com/voc-compliance-strategies/
http://www.directindustry.com/prod/brooks-instrument/product-14565-432127.html
https://www.pinterest.de/pin/382102349612248994/
http://www.agilent.com/home/more-countries?currPageURL=http://www.agilent.com/en-us/products/gas-
chromatography/gc-systems/490-micro-gc