Ceramics UK 2019 presentation

1. THE PULSATION REACTOR
Pushing the Limits of Particle Synthesis

2. 7/11/20192
CONTENT
COMPANY
APPLICATIONS
PULSATION REACTOR
▪ The Process
▪ Feed Materials
▪ Comparison
▪ Material Properties
▪ Ceramic Application
SUMMARYSUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

3. 7/11/20193
▪ Service provider
− Thermal treatment of client
materials
− Scale-up trials and production
▪ 16 rotary kilns & 8 pulsation reactors
▪ ≈170 employees at 2 locations
▪ 20.000 tons capacity a year
▪ Subsidiary of IBU-tec
▪ Metalorganic products:
− Organotin compounds
− Catalysts and glass coatings
− Intermediates
▪ ≈90 employees
▪ Chemical Park Bitterfeld-Wolfen
BNT ChemicalsIBU-tec advanced materials AG
Weimar
Bitterfeld
Nohra
140 km
Thermal Processing & Organotin Products
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

4. IBU-tec and BNT each focus on different steps
and unit operations in chemical production
7/11/20194
Organotin Chemistry & Contract ManufacturingThermal Processing Solutions
Processing in
Rotary Kilns /
Calciners
& Pulsation Reactors
• Oxidation
• Reduction
• Calcination
• Pyrolysis
DissolutionPrecipitation
Distillation
(Vacuum)
Agglomeration
Synthesis
(<250°C)
Mixing
Impregnation
Filtration
Grinding
Sieving
Drying Crystallization
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

5. Markets & Industries served
7/11/20195
Container Glass Coatings
Homogenous Catalysts
PVC Stabilizers
Heterogeneous Catalysts
Battery Materials
Building Materials
Proppants
Specialty Chemicals
Automotive Catalysts
Thermal Process Engineering & Organometallics
Group
High Performance Ceramic Precursors
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

6. The Pulsation Reactor
6 7/11/2019
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

7. The Pulsation Reactor
7 7/11/2019
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

8. 7/11/20198
→ Flame/Tube reactor with pulsating hot gas
stream for thermal shock treatment
→ Feed: powder, suspension or liquid solution
→ Operating Temperature range: 250-1300 °C
The Pulsation Reactor is a flame reactor based
on pulse combustion technology
MAJOR APPLICATIONS
▪ Production of catalytically
active powders
▪ Powders as ceramic
precursors
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

9. PR facilitates enhanced heat/energy transfer
to the particles
7/11/20199
RESIDENCE TIME
PARTICLE TEMPERATUREVELOCITY
→ Pulsating carrier gas flow leads to in-
creased relative velocity (gas vs. particle)
→ Particles can be heated up at higher
heating rates
RESIDENCE TIMEWith pulsation
Without pulsation
Particle velocity
Relative velocity
Gas velocity
Effective Value
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

10. Ideal for homogeneous treatment – Narrow
residence time distribution, flat velocity profile
7/11/201910
NUMBER OF PARTICLESVELOCITY PROFILE
→ Pulsation flattens velocity profile → Pulsation leads to a narrowing of
the residence time distribution
RESIDENCE TIME
With
pulsation
Without
pulsation With pulsation
Without pulsation
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

11. 7/11/201911
PR’s Process Parameters and comparison to
other thermal processing technologies
TYPICAL PARTICLE SIZE
→ Shorter residence times compared to commonly
used processing methods
AVERAGE RESIDENCE TIME
mins h
nm
µm
mm
d
PR PROCESS PARAMETERS
▪ Maximum Temperature:
1300 °C – High-temperature
reactor for up to 1600°C
available in 2020
▪ Residence time: 0,2–2 sec.
Extension possible
▪ Maximum capacity: 1-2 t/day
Numbering up instead of
scale-up
▪ Atmosphere: oxidative
Air ratio close to 1 possible
Tunnel
Kiln
Pulsation
Reactor,
Flame
Reactor
Fluidized
Bed
Rotary
Kiln
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

12. Possible Feed Materials and Applications
7/11/201912
Typical objectives of thermal
treatment in pulsation reactor
Product Possible
Applications
POWDER Drying
Calcination
Powder
(µm)
Ceramics
Pigments
Additives
Catalysts
SUSPENSION Drying
Coating (Core-Shell)
Calcination
Powder
(sub - µm - µm)
Ceramics
Pigments
Additives
Catalysts
SOLUTION Nanoparticle synthesis Powder
(nm - µm)
Ceramics
Catalysts
CosmeticsSUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

13. Compared to Rotary Calciner, PR materials
with higher SSA at same Processing conditions
7/11/201913
0
50
100
150
200
250
300
350
600 800 1.000 1.200 1.400
Temperature [°C]
Specific Surface Area [m2/g]
Pulsation Reactor
Rotary Kiln
Precursor: Al(OH)3 Feed: Powder Product: Al2O3
Higher SSA of (carrier)
materials increases
the chemical
reactivity of catalyst
BENEFIT
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

14. Higher SSA of (carrier)
materials increases
the chemical
reactivity of catalyst
Compared to Rotary Calciner, PR materials
with higher SSA at same Processing conditions
7/11/201914
0
5
10
15
20
25
30
35
600 800 1.000 1.200 1.400
Temperature [°C]
Specific Surface Area [m2/g]
Precursor: Ce(NO3)4 Feed: Solution Product: CeO2
Pulsation Reactor
Rotary Kiln
BENEFIT
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

15. BENEFIT
A highly active powder
with optimized purity
as a result of the short
residence time com-
bined with narrow
residence time
distribution
Precursor: Al(OH)3 Product: Al2O3
Short Residence Time facilitates high
selectivity towards active phases
7/11/201915
20 30 40 50 60
2 Theta [°]
Relative Intensity [a.u.]
Pulsation Reactor
Rotary Kiln
δ-Al2O3
α-Al2O3
Feed: PowderSUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

16. Precursor and Solvent Type will Influence
Material Properties
7/11/201916
A P P L I E D P R E C U R S O R S
Acetate Alcoholate Nitrate / Carbonate
Solvent Used Water Alcohol Water
Particle Size [nm] 5 - 50 5 - 40 1.000 - 20.000
Particle Form Sphere Sphere (rounded) Sphere, partially hollow
(TEM / FE-SEM) TEM TEM FE-SEM
Particle
Morphology
Particle Form
Schematic
Spec. Surface Area
BET-range [m2 / g]
20 - 80 40 - 150 5 - 20SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

17. PR nano ceramic powders sinter at lower
temperature than comparable materials
7/11/201917
100
800 1.000 1.300 1.500
Temperature [°C]
Relative change in length [%]
Pulsation Reactor product
Typical standard product
1.100 1.4001.200900
70
75
80
85
90
95
Production of material
with improved sintering
characteristics
(sintering completed
at lower temperatures)
BENEFIT
Precursor: Zr-/Mg-Acetate Feed: SolutionSUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED
Product: ZrO2/MgO

18. 7/11/201918
→ Pulsation reactor is a tube reactor with pulsating hot
gas stream for the THERMAL SHOCK TREATMENT
→ Increased heating rates facilitate HIGHER SPECIFIC
SURFACE AREA materials
→ Material with UNIFORM PROPERTIES is made possible
by the narrow residence time distribution
Summary
SUMMARY
CERAMICS
MATERIAL
COMPANY
APPS
COMPARISON
PR
PROCESS
FEED

19. Find us at Booth 1522
7/11/201919
For the development of
ceramics with new and
improved properties,
the pulsation reactor might
be the right technology.
THANKS FOR YOUR ATTENTION!

20. Nomenclature
7/11/201920