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Flow Chemistry and Microreactorsturn Process Performance

into Money?Continuous Flow Technology in Industry, York 2012

Dr. Dirk Kirschneck, Microinnova Engineering GmbH

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content

• efficient flow processing

• scale up & realization

• manufacturing systems

• flow miniplant systems

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specialists in process intensification

processdevelopment

engineering& plant

Microinnova combinesprocess knowledge

with plant competence

www.microinnova.com

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thermostat

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product

process intensification step by step

evaluation

plant

check

plant check report

step 1 milestone

potential

proof

verification

basic

feasibility

preliminary study

lab-scale plant

test matrix

step 2 milestone

basic

proof

development

technical

feasibility

device screening

critical parameters

parameter optimization

data for engineering

step 3 milestone

parameter

optimization

realization

engineering

& plants

scale up

plant design

engineering

construction

step 4 milestone

industrial

plant

turn-key-plant

efficient processing

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aim of micro innova

make chemicalprocessing

more efficient

2

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drivers for flow and/or microreactors

www.microinnova.com

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thermostat

product product waste

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gas

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product

towards perfect processing

• narrow residence time distribution• no backmixing• no hot spots

• ideal stoichiometry• no high concentration spots • no dead zones

perfectmixing

perfectmixing

perfectheat

exchange

perfectresidence

time

perfectheat

exchange

reactionzone 1

reactionzone 2

reactionzone 3

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process intensification toolbox

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example: selectivity increase

Friedl-Crafts-Alkylation

J. Yoshida, “Flash Chemsitry”, Wiley, 2008

driver

toolbox

0,00

0,25

0,50

6,06,07,5

9,0

0,75

4010,5

60

80

conversion

flow rate [ml/min]

concentration [g/l]

Design ofExperiments

restime

concentration

600500400300200100

80

75

70

65

60

55

>

–

–

–

–

–

–

–

–

–

<

0,61 0,67

0,67

0,13

0,13 0,19

0,19 0,25

0,25 0,31

0,31 0,37

0,37 0,43

0,43 0,49

0,49 0,55

0,55 0,61

selectivity

selectivity

restime

concentration

600500400300200100

80

75

70

65

60

55

>

–

–

–

–

–

–

–

–

–

<

0,94 1,00

1,00

0,46

0,46 0,52

0,52 0,58

0,58 0,64

0,64 0,70

0,70 0,76

0,76 0,82

0,82 0,88

0,88 0,94

conversion

conversion

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Hydrogenation of a polymer double bond

example: reaction rate enhancement

driver toolbox

Similar Reaction Residence Time Conversion

Macro-Batch 5 hours 100%

Flow-Reactor 2 minutes 100%

CH3

CH3

R

n

+ H2

Raney Ni

140°C/80bar

CH3

CH3

R

n

3

realization considerations

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target area

IdeaVerification

ScalableDevelopment

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heat release characteristics

Time

HeatRelease

Zone1 Zone2 Zone3 Zone4

Point ofMixing

t

1

t2 t3 t4

.Q1

.Q2

.Q3

.Q4

ProvidingPerfect

Environment for the Chemical

Reaction

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scale up of flow processes

Exothermityheat v time

Interfacearea v time

Mixingquality v scale

Plug flowquality v scale

Time

MixingQuality

Time

InterfacialArea

HeatRelease

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scale out concept

a) internal numbering up

b) smart dimensioningincrease

increase

increase

constant

increase

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scale up of flow processes

CorningAFR

Alpha LavelART

IMMCaterpillar

IMMStar-Lam

Flow Miniplant Level up to 10 l/hour

Manufacturing Level up to 10.000 l/hour

4

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comparison batch versus conti / flow

advantage batch• flexibility• multipurpose

process is adjustedto the plant

advantage conti/flow• process performance• safety

plant is adjusted to the process

concept necessary, which combinesbatch flexibility with continuous performance

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on-module flexibility

on-module adaption by exchanging specific parts

engineered spaces for adaption

residence-timemodule

reactor

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inter-module flexibility

feed 1 feed 2 feed 3 reactor 1 reactor 2 product

module storage

manufacturing solutionplant redesign

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plant redesign-concept

Kirschneck et al.; Chem.Eng.Technol. 2007, 30(3), 305-308

• starting point: one single process step

• integration of microreactors or micro-structured components

• interventions as small as possible

case study example:

• capacity: 3 tons/hour

• effect• double plant capacity

• energy savings

• investment costs: 1/10 compared to conventional

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first test run

5

manufacturing solutionunit operation

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unit operation - solution

• typical for one process step

• typical solution for inefficient or difficult process steps

• implements individual reaction steps in a continuous process

• no modification of remaining process steps

• dedicated or limited multipurpose

• on-module flexibility

• savings:

• higher yields

• less energy consumption

• less raw material input

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case study unit operation-concept

case study example:

• mixing-sensitive reaction

• barely feasible in batch mode

• microreactor plant results: 30 % higher yield compared to batch

• total throughput is 200 l/hour

• the pilot/production plant has been started up successfully in May 2010

• yield difference (lab-manufactur-ing): 0.1%

•

one of the biggestcGMP

plants withmicroreactor

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fast track realization

2009 2010

09

first lab-experiment launch of the plant at the customer site

case study example

10 11 01 02 03 04 05 0612

October 2009 May 2010

manufacturing solutionmodular multipurpose

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modular multipurpose-concept

• combines advantage of batch technology (flexibility ) with advantage of continuous processing (process per-formance )

• interchangeable modules temporarily assembled and variably combined

• functional units, which can be combined individually according to the process

• fast adaption to new processes and easy plant extension

• optimization of plant utilization

• totally new plant concept in chemical industry

6

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control room

modular multipurpose-concept

feed 1 feed 2 feed 3 reactor 1 reactor 2 product

utilities-hub

production area

tank farm

utilitiesautomation + supply

• bus /plc• electricity• control air• nitrogen

heating + chilling

module storage

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case study modular multipurpose

S

T

O

R

A

G

E

S

T

O

R

A

G

E

FEED 1

FEED 2

FEED 3

REACT1

REACT2

R

E

S

I

D

E

N

C

E

S

E

N

S

E

flow mini-planttechnology

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flow mini-plant

• link between development and manufacturing

• maximum flexibility by ready modular units

• simple adjustment to new processes

• easy operation

• freely selectable level of automation

• GMP or non-GMP kilo laboratory use

• applicable for small scale manufacturing

Development orientated:

S-Class 1-10 l/h

Manufacturing orientated:

M-Class 10-100 l/h

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Reaction moduleFeed module Product module

flow miniplant example

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automation concept flow miniplant

7

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flow mini-plant module examples

module examples:

liquid feed module with buffer tank

reaction module with plate-reactor

reaction module for 2 stepreaction and multi injection

gas feed module heating/coolingmodule

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summary

fast trackrealization

flexibility safetyprocessperformance

turning process performance into money

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Meet some people who make it happen

Dipl.-Ing. Walter Linhart, perfectionist“We set up modular manufacturing systems that will allow our customers to transfer their competences into productivity in the highest degree.

Dr. Günter Tekautz, puzzle freakYield and process stability increases to the same extent as the number of possible synthesis routes can be expanded by flow and other intensification technologies.

The research leading to these results has received funding

from the European Community's Seventh Framework Pro gramme

[FP7/2007-2013] under grant agreement no. CP-IP 228 853-2

Please contact me:

+43-316-908606-110

dirk.kirschneck@microinnova.com