New Offerings from Albemarle

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New Offerings from Albemarle John Parks Director Fine Chemicals R&D 1

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New Offerings from Albemarle Presentation

Transcript of New Offerings from Albemarle

Page 1: 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

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The Phase Diagram

LiquidMelting

ssur

e SolidEvaporation

Pre

s

Vapor

Sublimation

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Temperature

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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

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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

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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

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yield

Tsub

1015torr

Example dataset

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a p e dataset(No product degradation detected)

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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

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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

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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

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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

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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

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In Action

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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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