Educating the Customer: PI - What’s it all about?

Dr Mike Jones, Protensive

PROCESS INTENSIFICATION: Meeting the Business and Technical Challenges, Gaining Competitive Advantage

The Royal Institution of Great Britain, London: 19th November 2003

What is PI?

E q u ip m e nt P ro du c ts P ro ce sses E ffe c ts

P I

What is PI?

S m a lle rL ig h te r

C h ea p er

E q u ip m e nt P ro du c ts P ro ce sses E ffe c ts

P I

What is PI?

S m a lle rL ig h te r

C h ea p er

E q u ip m e nt

Im p ro vedN o ve l

P ro du c ts P ro ce sses E ffe c ts

P I

What is PI?

S m a lle rL ig h te r

C h ea p er

E q u ip m e nt

Im p ro vedN o ve l

L o w er co st

P ro du c ts

R e s ide n ce t im e

H e at tra ns fe rM a ss tra n s fe r

S e pa ra tionF lo w b e h av io ur

P ro ce sses E ffe c ts

P I

What is PI?

S m a lle rL ig h te r

C h ea p er

E q u ip m e nt

Im p ro vedN o ve l

L o w er co st

P ro du c ts

R e s ide n ce t im e

H e at tra ns fe rM a ss tra n s fe r

S e pa ra tionF lo w b e h av io ur

P ro ce sses

D e live ry sys te m sS u rfa ce e ffe c ts

F e e l

E ffe c ts

P I

Process Intensification - a definition

•Significantly enhances the transport rates

•Gives every molecule the same processing experience

CONCEPTS

- Match mixing/mass transfer rate to rate ofdesired chemical reaction

- Match heat transfer rate to exothermicity ofreaction (remove heat as it is produced)

- Match flow behaviour (eg plug flow, backmixed)to reaction scheme

- Match residence time to desired reaction time

A Reason

So rather than adapting the operating conditions and chemistry

to available classical equipment,

the process structure, architecture and equipment can be adapted to the physico-chemical transformation

What is PI?

E q u ip m e nt P ro du c ts P ro ce sses E ffe c ts

P I

SLUG FLOW

DROPLETEMULSION

PARALLEL FLOW

Diffusion between streams Diffusion in/out of droplets

Diffusion across the interface

Internal convective transportTypical Methods Typical Methods

for Contacting for Contacting Two Fluid PhasesTwo Fluid Phases

Channel Scale Channel Scale 5050m - 500m - 500mm

Scale-Up for Intensified ProcessesScale-Up for Intensified ProcessesFuture VisionFuture Vision

Low Volume Fine ChemicalsLow Volume Fine Chemicals

Several single channel devices with high flow velocity could Several single channel devices with high flow velocity could produce produce 10s of 10s of l/sl/s or around or around 1kg per day.1kg per day.

Medium Volume Chemical Medium Volume Chemical ProductionProduction

Blocks with Blocks with 1000s1000s of channels of channels running in parallel could provide running in parallel could provide higher yield higher yield whenwhen accurate accurate manifold technology developed.manifold technology developed.

COMBUSTION

CATALYST

PROCESS

CATALYST

COMBUSTION GAS

(CH4 + AIR)

PROCESS GAS

(CH4 + H2O)

A pair of adjacent channels in the catalytic plate reactor showing the coupling of an endothermic reaction (Methane Reforming)

with an exothermic reaction (Methane Combustion)

Comparison of the Productivity of Different Reactors

Reactor ReactorVolume

Yield of C5+kg/m3/hr

Sasol 432 .1 29.98

Exxon 23.8 43.84

Plate Reactor 1.0 163.12

Electrolytic flow cells

CEM

Na2SO4

Na+

H+

SO4-2

Na2SO4H2S04 NaOH

NaOH

OH-

Liquid Film

Solid Surface

Micro Mixers

Influence of Surface WavesInfluence of Surface Waves

Typical raman spectra taken from SDR.

8000

6000

4000

2000

0

540 560 580 600 620

FTIR ATR bulk polymerization of styrene FTIR ATR bulk polymerization of styrene

0.00

0.02

0.04

0.06

0.08

0.10

Log

100

200

300

400

500

min

2800 3000 3200

cm-1

FT-NIR following a polymerizationFT-NIR following a polymerization

0.0

20.0

40.0

60.0

80.0

100.0

120.0

0 100 200 300 400 500

Time (min)

Co

nve

rsio

n (

%)

(ppm)1.01.52.02.53.03.54.04.55.05.56.06.57.07.5

Styrene proton signals all but gone

Polymerization evaluated by 1H NMRPolymerization evaluated by 1H NMR

OH

trans-Pinocarveol

trans-Sobrerol

OH

OH

OH

trans-Carveol

p-Cymene

O

Pinol

O

-pinene oxide

O

campholenic aldehyde(2,2,3-trimethyl-3-cyclopentenacetaldehyde)

H +H2O/H +

- H2O- 2 H2O

N(Et)2

via cis-Sobrerol

Main products from the rearrangement of -pinene oxide

ACatalyst

B

Rearrangement reaction; A – -pinene oxide, B – campholenic aldehyde

ACat.

B

F

E

D

C

D

K

J

I

H

Simplified reaction paths, where B is the wanted product (campholenic aldehyde)

Control•size•size distribution•form•coating

Applications•Pharmaceuticals•Electronics•Inkjets•Semiconductors

Why?

Performance of SDR Process

0

10

20

30

40

50

60

70

80

90

100

0 20 40 60 80 100 120 140 160 180 200 220

Time (mins)

Co

nv

ers

ion

(%

)

VISCOUS LIQUIDS e.g. POLYMERISATION

- 75% yield after 4 hrs- 25% unreacted starting material

recycle, reprocess

On-Disc Monitoring of CaCOOn-Disc Monitoring of CaCO33 Production Production

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

800rpm, 5ml/s

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

800rpm, 5ml/s

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

400rpm, 5ml/s

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

400rpm, 5ml/s

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

400rpm, 10ml/s

0.0

0.2

0.4

0.6

0.8

1.0

1.2

1.4

1.6

0 2 4 6 8 10 12 14

Radius (cm)

Ca(

OH

) 2 C

on

cen

trat

ion

(g

/lit

re)

400rpm, 10ml/s

• Probes mounted on disc surface to monitor ion depletion.

• Results confirm particle production is mass transfer limited and takes place on the spinning disc.

Examples of film thickness measurements made using this system.

Film thickness typically is in the 0.01m to 1mm range.

Real-Time Film Thickness Monitoring

Liquid-Solid Mass Transfer Results

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0 5000 10000 15000 20000

Shear Rate (1/s)

Ma

ss

Tra

ns

fer

Co

eff

icie

nt

(mm

/s) 38ml/s

21ml/s

10ml/s

6mm Electrode - 200 to 900rpm

Diffusion Theory Prediction

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0 5000 10000 15000 20000

Shear Rate (1/s)

Ma

ss

Tra

ns

fer

Co

eff

icie

nt

(mm

/s) 38ml/s

21ml/s

10ml/s

6mm Electrode - 200 to 900rpm

Diffusion Theory Prediction

Results for 6mm Electrodes at 9 Radial Locations

Summary

• Rapid process screening

• Rapid process development

• Rapid scale-up• Novel products and

processes• JIT

• Integrated processes• common standards