New Offerings from Albemarle
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Transcript of New Offerings from Albemarle
New Offerings from Albemarleg
John ParksDirector Fine Chemicals R&D
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SublimationWhatWhWhyHow
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The Basics about Sublimation….
• Sublimation is when a substance transitions from the solid phase directly into the gas phase
• Most substances require reduced pressure to sublimeMost substances require reduced pressure to sublime• Like boiling, sublimation can be used as a way to separate and purify
different compounds• One rule of thumb is the greater molecular weight differences g g
between substances the easier it is to separate them using sublimation
• Common sublimation techniques include: simple vacuum bli ti t i t bli ti d f ti l bli tisublimation, entrainment sublimation, and fractional sublimation
The Phase Diagram
LiquidMelting
ssur
e SolidEvaporation
Pre
s
Vapor
Sublimation
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Temperature
Why Use Sublimation?V Di till ti• Versus Distillation
• Lower temperatures (temperatures around melting point instead of boiling point)
Avoids undesired reactions:• Avoids undesired reactions:• Polymerizations caused by high temperatures• By-product formation• Decompositioneco pos o
• Versus Crystallization• Useful for low soluble /high purity material
• Metal-organics• Large organic molecules
Sublimation at the Process Development Center (PDC)( )• Two different labscale setups have been built and tested
• Simple vacuum sublimation• Nitrogen entrainment sublimation
• Two different molecules have been screened using sublimation• AlQ3 and a proprietary molecule
Vacuum Pump
Simple Lab Sublimation Unitp
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Rev 1 cold finger
Flask type, lots of area Body – note crust
Widest part of coldfingeracts as a heat sink, cooing the body and promoting condensation
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Rev 2 coldfinger
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Coldfinger type effects
Flask type Finger type
A bit hard to see butA real reduction of crustOn the wall
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Use simple setup as a screenSurface Plot of yield vs Tsub, torr
Note strong dependence
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Note strong dependence On pressure AND temperature
0
20
40
5
350
300
40
350
450
00
yield
Tsub
1015torr
Example dataset
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a p e dataset(No product degradation detected)
Example 2 Compound X
• Impurities in X• X (substrate)• Di substituted XDi substituted X• Tri substituted X
• Goal• Goal• Separate the X from the Di and Tri substituted compounds in an
acceptable yield
High Vacuum Sublimation SystemSpecialized High Vacuum valves and iinstruments
Sublimation Fl k
Vacuum Manifold
Flask
Cryogenic trap
Hot Oil Bath
Diffusion Pump
Vacuum Controller
High vacuum hose to roughing pump
Simple Sublimation Comp X
• Setup includes a hot oil bath, sublimation flask with internal condenser, and a vacuum pump
• Maximum operating conditions:Maximum operating conditions:• 1 mmHg• 200 C oil temperature
• Note Modest conditions
Simple Sublimation Summary
• Best results occurred at 1 mmHg and around 100 C
• Concentrated X by 100 to 150Concentrated X by 100 to 150 area%
• Reduced di-substituted X by around 40 area%
Condenser
around 40 area%
Residue after sublimation
Condenser sample
Entrainment Sublimation
• Use hot inert gas • Allows sublimation to occur at higher pressure• Very important for those products that need ultra deep vacuum• Very important for those products that need ultra deep vacuum
• Vacuum pump cost• Energy cost
M i t d d t k t l d• Maintenance needed to keep system sealed
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Entrainment Sublimation
Exhaust filter Thermocouple measuring temperature in sublimation chamberSublimation
Screening Unit
Condenser
Use to test feasibility
Sublimation chamberSet initial conditions
Preheated gas feed to chamberPreheated gas
feed to jacket
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Entrainment Sublimation of AlQ3
• Scale up system for production of AlQ3
• Feed preheat sublimeFeed, preheat, sublime, deposit in semi-continuous mode
• 5-10 kg/day5-10 kg/day
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Working Unit
Condenser
Gas Preheat
Collection Flash
Fluid bed
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Sublimation Chamber
In Action
Albemarle FCS Research & Development
• 50 Chemists and Engineers
• Support the Business• Support the Business• Route Development• Process Scaleup
E i A l i• Economic Analysis
• Develop New Technology• Continuous Reactor Lab• High Throughput Labs• Sublimation Lab
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Albemarle Fine Chemistry Services
• Custom Manufacturing• Pharma• Agg• Electronics• Renewables
• Huge Capability Span• Huge Capability Span• 10s of kgs to 10’s of millions of kgs• Proven capability
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