Advanced Process Technology Shared Innovation Program Provide! · PDF fileAdvanced Process Technology Shared Innovation Program Provide! ... Advanced Process Technology Shared Innovation

Advanced Process TechnologyShared Innovation Program Provide!Overview of technical program lines

Shared Innovation program lines

Small-scalededicated production

Flexible & scalablemultipurpose continuous

Versatile programmableFormulation systems

a) Small scale continuous flow processing

b) Highly selective separation concepts

c) Electrochemistry & external field enhanced

d) Handling & processing of complex fluids

e) Modularity, flexibility & asset-light

Cases from industry

Technologies/tools from partners (equipment, academica)

Advanced Process Technology Shared Innovation Program Lines

2

A) Reactor Technology“Demonstration of reactors for challenging processes”

L.F.G. Geers, J. Urbanus

Properties & options of continuous reactor technology


4

Reactor Technology: Impact & Focus


Impact:

Improved product quality in terms of yield, selectivity and product concentration

(reduces use of solvents)

Scalability of process equipment to reduce development time (easier

translation from lab to pilot), shorten time to market, and to facilitate variable

production sizes (for volatile markets)

Focus:

Flexibility of products for volatile demand/supply & variety of consumer

interests

Reduced costs of equipment modules to compensate loss of economy of

scale when numbering up

5

Visionary goal & TNO focus


2020-2030

enabling

Functionality manufacturing

2050

2 main topics:

- Multiphase (solid-liquid) processing

- Strongly exothermic processes

Miscellaneous:

nano-particles, highly-viscous media

source: www.lonza.com

6

State-of-the-art outside TNO


F3 factory (FP7 project)Goal : Development of plug&play modular equipment & holistic design methodology

Flow mini plant (Micro Innova)Modular design combined with process intensification technologies provides efficiency and flexibility.

Chemtrix / ESKDevelopment and consultancy on scalable modular continuous flow equipment

FLOWIDLab scale development platform for fast and easy modular process development

7

State-of-the-art at TNO


Industrial scale installation(Zeton & TNO for Solvay)

CoRIAC : demonstration of flow chemistry on lab, bench and pilot scale

DiMeCo : dissolving metals in a continuous flow process

Flow4API : screening chemistry to optimize for flow chemistry and telescoping, and demonstration on production scale

8

TNO Helix® reactor

Potential industrial applications of (TNO)continuous reactor technology

Solid-liquid processes

Heterogeneously catalysed reactions (hydrogenations, formylations)

Reactions with solid reagents or products (organometalics, pharmaceuticals

production)

Nano-materials production

Highly viscous liquids

Dangerous chemistry

Novel process windows (high pressure & temperature)

Production of energetic materials


Twin screw extruder (source: TNO)

Oscillating baffled crystallizer (source:TNO)

9

Next steps - What would we do with 500 kEUR?

Demonstrate continuous reactor technology for new challenging cases:

… construct a flexible skid in which modular systems can be assembled

… consisting of process modules with reactors, feed sections, product sections

… including process monitoring and control system for in-line product quality

assessment

Develop/improve/apply innovative reactor modules:

… for heterogeneous processes (especially solid-liquid, but also gas-liquid)

… with alternative energy sources, e.g. ultrasound, microwave, photochemistry,

etc. to demonstrate and evaluate their applicability

… for highly viscous media, e.g. using extrusion

… with integrated separation of products or by-products

… with multiple feed points along the reactor, e.g. for telescoping reactions


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B) Modular Separation Technology“Translating principles to proven modules”

C.P.M. Roelands, J. Urbanus

2020-2030

enabling


2050

PROVIDE! – Modular Separation Technology


General concept: separation as integral part of the modular process system

12

Higher operating margins desired for EU for (fine)chemical industry:

a. Lower operating cost - expressed in:

- lower PMI [kgfeedstock+auxiliairies /kg product]

- lower E-factor [kgwaste/kg product]

- lower E-consumption [kWh/kg product]

b. Lower capital cost - lean infrastructure

for distributed / localized production,

utilizing renewable energy & feedstock:

- modular flexible equipment

c. Higher income on products:

- improved product quality (purity, particle size)

- higher added value products

improved mass & energy efficiency => also less equipment needed

Key role for Separation TechnologyInnovations

boundary condition for technology

opportunity to integrate separation with product forming


Modular Separation Technology: Focus & Results

13

Potentially relevant topics for industrial cases


1. Integrated reaction / separation :

- to improve overall yield /productivity

2. Highly selective separations:

- recycle of unreacted feedstock

- recovery of auxiliaries (e.g. catalyst)

- removal of similar byproducts

- separation of enantiomers

3. Solvent switch / swap between two steps:

- for solutes and for particles

4. External field driven separations

- to enhance separation efficiency

- to use renewable energy

5. Separation from highly viscous systems

- lifting mass transfer limitations

6. Integrated separation / particle formation

- in one step right size, structure,

shape

1. 2.3. 4.

5. 6.

reactor 1 separation 1

feed A

feed B

recycle

product

purge

formulation

feed C

reactor 2 separation 2

recycle

purge feed D

Objectives:• To build industrial case based program for development of modular separation

technologies (toolbox will be filled gradually)• To connect industrial cases with technologies from (SME) equipment manufactures• To demonstrate advantages for industrial cases at bench scale

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Principle

for

Separation

Integrated

Reactor /

Separation

In-line

separations

Solvent switch

/ swap

External

field assisted

separation

High viscosity

separations

Integrated

Separation /

Formulation

Vapour

pressure

Falling film

evaporator

Flash evaporator

/ Microsieve

Spray

evaporator

Rotating

Packed Bed

Spray

Crystallization

Solvent

affinity

(dissolved)

Pulsed Packed

Column

Membrane

Contactor

Spinning Disc

Contactor

Solvent

affinity

(crystal)

Oscillating

Baffled

Crystallizer

Hydraulic

Wash Column

Crystel /

Ultrasound /

Electrospray

Pulsed Helix

mild shear

crystallizer

Surface

affinity

Pervaporation

/ Ligands

Organophilic PV

/ SMB

Electro

Dialysis

Template

Induced

Crystallization

Molecular

size

Size Exclusion

Chromatography

Organic

Solvent

Nanoniltration

MATCH methodology to select appropriate separation technology for a specific industrial case


15

6 examples of potential developments (2)


Integration Reaction + Separation:

Pervaporation of reaction waterIn-Line Separations:

Membrane extraction from suspension

Solvent switch:

Flash evaporator

Field enhanced separation:

in-situ electrochemical crystallizationHigh viscosity separation:

HiGee/HighShear equipment

Integration Separation + Particle formation:

Pulsed Helix® for cooling crystallization

Illustration of options for research possible within Provide!Actual research topics depend on industrial cases of participants

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Partners on separation technology1. Universities

(discovery and early stage technology development)e,g, TU Dortmund, TU/e, TU Delft, UT, WURC

2. SME Equipment manufacturers(develop and launch technology) e.g. Pervatech, Solsep, TOP, Evodos

3. Equipment manufacturers (sell and manufacture proven technology) e.g. Sulzer, GEA

4. Engineering Consultants / Contractors (select proven technology for implementation)e.g. PDC, Avantium, Novasep, Traxxys

5. R&D departments large companies (select technology for piloting and implementation)e.g. DSM, AkzoNobel, GSK

6. Plant technologists (implement technology)


17

Principle

for

Separation

Integrated

Reactor /

Separation

In-line

separations

Solvent switch

/ swap

External

field assisted

separation

High viscosity

separations

Integrated

Separation /

Formulation

Vapour

pressure

Falling film

evaporator

Flash evaporator

/ Microsieve

Spray

evaporator

Rotating

Packed Bed

Spray

Crystallization

Solvent

affinity

(dissolved)

Pulsed Packed

Column

Membrane

Contactor

Spinning Disc

Contactor

Solvent

affinity

(crystal)

Oscillating

Baffled

Crystallizer

Hydraulic

Wash Column

Crystel /

Ultrasound /

Electrospray

Pulsed Helix

mild shear

crystallizer

Surface

affinity

Pervaporation

/ Ligands

Organophilic PV

/ SMB

Electro

Dialysis

Template

Induced

Crystallization

Molecular

size

Size Exclusion

Chromatography

Organic

Solvent

Nanoniltration

MATCH methodology to select appropriate separation technology for a specific industrial case

Advanced Process Technology Shared Innovation Program LinesHalf a Million Euro to spend

Continuous separations

for integrated modular systems

Enhanced continuous separations

(fields,higee,

hybrids)

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C) Electrochemical production

Towards electrification of the chemical industry

The applications of electrochemistry


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Incentives for employing organic electrosynthesis

Organic electrosynthesis has the following advantages amongst others1,2:

Elegant control of reaction rate

High selectivity

High efficiency

Ease of automation

Green methodology

The use of pollutant free electrons as reactant

Reactions conducted at ambient pressure and temperature

Low emission of toxics

Electrolysis is modular

Possibility of flexible employment

1 Schäfer H.J., C.R. Chimi 14 (2011), 745-7652 Schmidt V.M. Elektrochemische Verfahrenstechnik (2003)


21

Example 3 of conventional vs. electrochemical production of p-methoxy benzaldehyde

Activation by chlorine: Electrochemical activation:

Advantages:

Avoiding use of toxic chlorine, lower operating temperatures, no

byproduct (HCl) formation3 Steckhan et al., Chemosphere 43 (2001), 63-73.


22

Electricity market developments

Present situation of centralised electricity production:

Trend towards renewable electricity production:

Fluctuations of electricity prices

ascribed to renewable energy4.

Renewables only accounts for 16.4%

of Germany’s electricity production

in 20095.

4 Fanone et al., Energy Economics 35 (2013), 22-345 Bundesministerium, für Umwelt, Naturschutz, Bau und Reaktorsicherheit

coal, oil, gas

wind / water

sun

thermal mechanical electrical

mechanical electrical

electrical


23

Exploitation of low and negative electricity prices

Exploitation by electrochemistry

Electrochemical energy storage systems are suggested for balancing

supply and demand but are relatively costly

Electrochemical synthesis can profit from low electricity prices

Typical electricity consumption:

Large scale (chlorine production): 43% of CAPEX

Fine and specialty chemicals: 13% of CAPEX


24

Research path for electrochemical applications (1)

Determination of the technical feasibility of the proposed electrochemical system by electro-analytical methods.

System

TEMPO = 2,2,6,6-tetramethylpiperidine-1-oxyl

Lab- / bench scale

Reactor design

Does electrochemical production meet the economical and technical requirements such as product concentration, current density, current efficiency, ….?

Development of an electrochemical reactor to handle the selected electrode materials and fluids amongst others


25

Research path for electrochemical applications (2)

Process

Economics

Piloting

Integration of the electrochemical reactor in an envisioned process. Focus on product separation and electrolyte recycling.

Determination of optimal economic conditions of the electrochemical process

Validation of the electrochemical process together with parametric research for model validation


26

Envisioned objectives

Work out cases for electrochemical technology including downstream

processing such as:

Ethylene oxide or ethylene glycol production

Paired electrosynthesis of propylene oxide

CO2 utilisation by electrochemical reduction

Production of fine chemicals / specialties such as ….

Development of generic electrolyser technology which can handle

different type of electrode materials

liquids and gasses

Integrate electrolyte models to enable down-stream process estimations

Incorporation and/or development of electrolyte models

Description of unit-operations standard not present in flowsheet progs


27

D) Handling & production of complex fluids

Processes and processing towards industrial (nano)-specialities, composites and heterogeneous catalysts

Context – processing of complex fluids

The nano-promise: control of dimensions in the nanometer regime

leads to outstanding product properties.

Processing routes

1. Top-down (physical means of size-structuring, such as milling,

spraying, etc).

2. Bottom-up (clever chemical routes, self-organisation, NP growth)

TNO takes its role when it comes to adapting scalable instrumental

techniques, equipment and processes from other industries

TNO wants to develop academic recipes into scalable processes by

using scalable setups, a nanoparticle pilot production plant and

making use of new-to-develop in- and on-line QC instrumentation


29

Top-down processing: printing techniques

Drying resultsConventional process (swirl flow nozzle)

Printing powder process (Rayleigh break-up nozzle)

Improving the product quality of dried dispersions by adapting industrial style inkjet printing heads for spray drying technology


30

Top-down processing: printing techniques

Drying resultsConventional process (swirl flow nozzle)

Printing powder process (Rayleigh break-up nozzle)

To be used in solvent swapping?


31

Top-down processing: printing techniquesTNO Encapsulation Printer

New processing technology for microencapsulation:

Generate core droplet by inkjet technology

Encapsulation by a liquid film / curtain of shell material

Formulating encapsulated micron-sized beads by custom-made printing setup


32

Bottom-up approach

Using novel colloid synthesis routes from academia and adapt them for

scalable setups:

• Towards continuous nanoparticle synthesis (Quality/scalability

improvement)

• Towards in-line and on-line QC (using partly in-house developed

ultrasound and light scattering tools)

• Towards integrated down-stream processing

Focus on: batch->continuous, controlled shear fields, in-line quality

control and automized downstream processing

continuous reactors, in-line analytics, integrated downstream processing


33

State-of-the-art

Off-line quality control using electron DLS, electron microscopy,

reology, mechanical stirrers

At TNO: we are building up in-line sizing and aggregation state

measurement tools, continuous reactors, scalable shear fields (static

mixers)

Our focus on scalability, repeatability and precision


34

Nanomaterials developmentfor Chemical and High tech Industries

Expertise on sol-gel, mineral, metal, polymer, hybridsNucleation and growthHybridizationSurface modifications

‘hollow’ silica beads Quantum dots

Ag- wires

Lanthanide Nanodot tracers

Homemade nano-titania-filled translucent resist for NIL

Photonic crystals


35

F) Modularity, flexibility and asset-light“Facilitate profitable modular processes”

I. Hernandez-Mireles, D. Verdoes, J. Urbanus

2020-2030

enabling


2050

Supporting tools & technologies


Modular components

Mainframe • Modular reactors• Modular separations

3 main topics:

- Module manufacturing

- Modular infrastructure

- Systems, models & tools

37

Supporting Technologies & Tools: Enablers & Results


EnablersEnablers

Manufacturing technology

Adv. sensors and controls

Adv. Systems modelling

and logistics

Adv. Modular reactors

Modular separation technology

Continuous & multi-purpose

processes

These enablers will result in:

- Localized production, utilizing renewable energy & -feedstocks

- Reduction of equipment cost per unit produced

- Decreased energy consumption & waste production

- Improved product quality- Minimization of operating labour- Less investment risks for

developing markets through scalable technology

- Flexibility for volatile demand/supply & variety of consumer products

38

Some flavours of module manufacturing


Module manufacturing:

Automated manufacturing

Innovative manufacturing

Throw-away principles

3D printing

Source: TNO

printing of conformal µ fluidic channels

Sartorius Stedim Biotech S.A.

Single-use reactor bags

ADMATEC

39

Automated manufacturing: 3D printing

Advantages for 3D printing

reactors

Tailored shape and size

Integrated functions, i.e.

catalyst contained in

material


Cronin L. Nature Chemistry Volume: 4, Pages:349–354 2012

3D printing on different materials

Plastics (reactors, prosthesis/implants)

Concrete (houses)

Ceramics

Food

…. In the future: metals

WinSun Decoration Design EngineeringCornucopia, MIT

40

Innovative manufacturing: membrane welding techniques


TNO

Membrane modules can be used in a

broader range of operating conditions

High temperature

High pressure

New applications need to be

developed to exploit these features

and manufacturing techniques

41

Some flavours of modular infrastructure


BAM.de - Sensor node of a self-configuring wireless sensor network

TNO/SPIRE1 – fouling & rheology sensors

Modular infrastructure:

In-line PAT sensors

New sensors (rheology, fouling)

Remote operation

Plug & play mainframe

42

Some flavours of systems, models & tools


Systems, models & tools:

Sustainability

Logistics and systems

Decisions support tools

MATCH

Technology

Chemistry

Electricity to chemistry

Resource efficiency

Bio-based economy

EU - DIMENSIONS

TNO-VITO-GCC

43

Next steps – What would we do with 500 kEUR?

Focus on innovative manufacturing methodologies � 3D-printing

Explore possible specifications/properties of printed reactor modules

Reproducibility of performance

Recycling of reactor material

Investigation of business models & business cases


Production output 1 (years 3-7)

Production output 2 (years 8-12)

Production output 3 (years 13-…)Stick-built plant capacity

t

Q

1st module

2nd module

3rd module

44

More information?Please contact:

Ir. Martijn P. de GraaffBusiness Line [email protected]+31 (0)88 866 6437+31 (0)6 222 608 71

Ir. Peter WolfsMarketing & Sales [email protected]+31 (0)88 866 5645+31 (0)6 222 607 63

Dr. Jean-Marie BassettBusiness Development [email protected]+31 (0)88 866 8118+31 (0)6 104 804 73

TNO Sustainable Chemical IndustryBusiness Line Enhanced ProcessingLeeghwaterstraat 462628 CA Delft


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