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www.vtt.fi FROM AN IDEA TO THE FINAL PRODUCT Scale-up with VTT

FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

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Page 1: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

www.vtt.fi

FROM AN IDEATO THE FINALPRODUCT

Scale-up with VTT

Page 2: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

BUILDING PARTNERSHIP THROUGH INNOVATIONS

The pilot plants are located in Otaniemi and Rajamäki near Helsinki. The total plant area is 1500 m2 of which 300 m2 is Ex-classified. We offer a unique combination of pilot scale reactors and downstream processing units.

WE CAN HELP YOU IF

a theory needs to be testeda synthesis needs to be optimizeda process needs to be scaled upa process needs to be optimizedempirical production data is required for the design of a new planta product is required for test-marketing purposesyou do not have the personnel or equipment to do it all yourself

•••••

SCALE-UP WItH Vtt

VTT´s pilot plants have excellent facilities for fast and efficient product development. The facilities are multi-purpose with a wide variety of reactors and downstream processes.

Health, safety and environmental issues are integral part of our daily work. We are experienced in handling a wide variety of chemicals. We serve customers from polymer, specialty chemical, food, paper chemical, coating and pharmaceutical industries. We also carry out process development and scale-up services to help our clients commercialize new products.

Rajamäki pilot plant

Otaniemi pilot plant

WE WELCOME NEW CHALLENGES

VTT is your partner in developmentin your business.

VTT is an impartial expert organisation that carries out technical and technoeconomic research and development work. We also offer information services. VTT is a contract research organization involved in many international assignments. With its more than 2700 employees, VTT provides a wide range of technology and applied research services for its clients, private companies, institutions and public sector.

Page 3: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

MULtIPURPOSE REACtOR SYStEMS

VTT´s two reactor systems provide excellent possibilities for several industrial applications. Synthesis, polymerizations and product modifications of wide temperature and pressure ranges can be performed with the multipurpose reactor systems having capacities between 160 and 1800 dm3. Our glass-lined reactors are specially suitable for fine and speciality chemical synthesis. Example processes include esterifications, etherifications, hydroxy alkylation, condensation and radical polymerisation, oxidation, chemical and enzymatic hydrolysis. We have special expertise in biomass fractionation and modification. Reactors are equipped with extensive control and data collecting system.

Glass-lined Stainless steel

Volume (dm3) 160 500 395 474 1800

temperature max (°C) 170 150 300 300 200

temperature min (°C) -25 -10 0 0 -50

Pressure max (bar) 6 6 50 50 13

Pressure min (mbar) 10 10 10 10 10

Ex-classified x x x x x

MULtIPURPOSE REACtOR SYStEMS

Page 4: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

SPECIAL REACtORSSeveral reactors suitable for all kinds of synthesis

Büchi steel reactors from 0.5 to 10 dm3

Büchi glass reactors from 1 to 60 dm3 Tube reactor for cold synthesis (69 kW cooling system)Steel reactors from 20 to 600 dm3

These special reactors can be operated over a wide range of temperatures and pressures (-35… +250 °C, 10 mbar…60 bar).

For example, we can offer a 430 dm3 steel reactor with helical mixer for viscous materials under pressure or vacuum, and a 250 dm3 reactor/ dryer for products with wide range of particle size and solid content.

For safe scale-up of the synthesis, knowledge of reaction heat is essential. It can be measured

•••

with Mettler Toledo RC1W reaction calorimeter at up to 100 bar pressure. The calorimeter is also equipped with on-line FTIR-probe to monitor chemical composition.

Büchi 60 dm3

Drais Turbu Dry 250

430 dm3 steel reactor

Helical mixer of 430 dm3 reactor

Reaction calorimeter

Page 5: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

SEPARAtIONS AND FILtRAtIONS

Pilot plants are equipped with versatile downstream process units for liquid/solid separations and efficient product recovery. Also flammable solvents can be handled safely.

SEPARAtION EqUIPMENt

Technical data:

Larox VF8 Alfa-laval Clara-80

Alfa-laval NX-309-B Seitz terra EF60/250

Alfa-laval NX-309-B

Westfalia SB 7-36-076

Alfa-laval Clara-80

Larox VF8/1,0

PCI P1 Pall hollow SLP-3053

Millipore ceramic

Seitz zenit V40/14

Seitz terra EF60/250

Decanter centrifuge

Clarification separtor

Clarification separtor

Rotary vacuum filter

Crossflow utrafilter

Crossflow ultrafilter

Crossflow microfilter

Plane and frame filter

Filter

Filter (m2) 1.0 1.0 4.5 0.2 2.0 0.28

Capacity (m3/h)

0.1...1.5 0.1...1.0 0.1...10 0.2...2.5 0.01...0.03 0.2 0.01...0.03 1...3 (volume 230 dm3)

Solid cont./ feed (%)

0...30 0...3 0...5 0...30 0...30 0...20 0...20 0...20 0...50

Ex- classified

x x x x x x x

Page 6: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

DIStILLAtION AND EVAPORAtION

Conventional and vacuum distillations can be carried out in multi-purpose reactor systems.

For small-scale distillations we have vacuum fractional distillation units with packed columns up to 30 theoretical plates and adjustable reflux ratio.

Evaporation can be performed by using falling film evaporator or vacuum contact dryers. The falling film evaporation technique is suitable for concentrating heat sensitive products. The capacity of the evaporatorranges from 30 to 300 dm3/h at a temperature

Distillation unit with packed column Falling film evaporator

range of 0 - 90 °C. The equipment is ex-classified.

GFT Pilot unit: fluid separation system by pervaporation membrane. A specific component in a feed mixture passes through a membrane by a solution-diffusion transport mechanism. Membrane area is 13.5 m2. Capacity for example; ethanol 94 w-% to 99.5 w-%, 17 kg/h. The GFT Pervaporation membrane is ideal for use in the dehydration of organic mixtures and in the extraction of organics from water.

Page 7: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

DRYING

The drying process is often the final step in product manufacturing. The drying method is selected according to the properties of the feed and the requirements of the final product. We have several dryers at our disposal, such as fixed bed dryer and vacuum contact dryers.

Rajamäki pilot plant offers spray drying possibilities for liquids, suspensions or particle slurries into powders using atmospheric air as a drying medium. The drying capacity of Niro P-6.3 spray dryer is 30 - 50 kg/h depending on the drying temperature and solid content of the feed. The product temperature range is typically between 70 and 100°C.

Contact drying is a very effective drying method for a wide range of products. Drais TurbuDry TD 250 can be used for reactions, evaporations, compacting and granulation of materials, mixing, dispergation and coating. The advantages are short drying time and low drying temperatures, which also make it very suitable for heat sensitive materials. The equipment can master the phase change from pasty to crumbly product without problems.

Drais tD250 Lödige Vt50 Lödige M20 Karix II Seitz terra EF60/250

Vacuum contact dryer

Vacuum contact dryer

Vacuum contact dryer

Fixed bed dryer Vacuum contact dryer

Volume (dm3) 250 50 20 800 230

temperature (°C) -10...200 -10...158 -10...158 -10...65 -10...150

Mixer (P/kW) 15 2.5 1.5

Mixer (rpm) 15...135 200 100 32

Homogenizer (P/kW) 9 2.7

Homogenizer (rpm) 1500...3000 1500...3000

Ex-classified x x x

Niro spray dryer, P-6.3 Drais TD250

DRYERS tECHNICAL DAtA

Page 8: FROM AN IDEA - VTT - Teknologiasta tulosta · for the design of a new plant ... MULtIPURPOSE REACtOR SYStEMS ... falling film evaporator or vacuum contact dryers

For more information

Rajamäki pilot plant:Mika Härkönen, Senior Research Scientisttel. +358 20 722 [email protected]

Pertti Tiitola, Research Engineertel. +358 20 722 [email protected]

Otaniemi pilot plant:Tuulamari Helaja, Senior Research Scientisttel. +358 20 722 [email protected]

Pia Willberg-Keyriläinen, Research Scientisttel. +358 20 722 [email protected]

VTT TECHNICAL RESEARCH CENTRE OF FINLANDVuorimiehentie 5, EspooP.O. Box 1000, FI-02044 VTT, FinlandTel. +358 20 722 111, fax +358 20 722 7001www.vtt.fi

• VTT is the largest multitechnological research organisation in the Northern Europe • VTT develops new technologies, creates new innovations and value added thus increasing customers’ competitiveness • VTT produces research, development, testing and information services to companies and public sector •

SUMMARY OF Vtt PILOt PLANt FACILItIES

Reactors

• Two multi-purpose reactor systems: 160 dm3…500 dm3, glass-lined 250 dm3…1800 dm3, Avesta SMO• Several other reactors 0.5 dm3…600 dm3 Steel, Glass, Hastelloy Temperature range: -50...+300 °C• Pressure range: 10 mbar…60 bar• Reactors for viscous and corrosive materials• Drais reactor (reaction, distillation, drying, granulation, dispersion)• Tube reactor

Distillation• Conventional and vacuum distillation in reactor systems and separate distillers• Falling film evaporator (water 50 dm3/h, suitable also for organic solvents)• Distillation unit (packed columns, vacuum, adjustable reflux ratio)

Solid handling• Filtration: Plane and frame filter (2 m2), rotary vacuum filter (1 m2), pressure bag filter, Nutsche filter (0.28 m2)• Clarification separators (feed max 10 m3/h)• Decanter centrifuge (feed max 1.5 m3/h)• Fixed bed dryer (0.8 m3), vacuum contact dryers (50 dm3, 230 dm3, 250 dm3)• Wet and dry mills• In-line mixer (Ytron Z60)• Materials AISI 316

Other process possibilities• Reaction calorimeter (100 bar)• Ultrafiltration (0.5+1.0+4.5 m2)

• Pervaporation (for example ethanol 17 kg/h)• Advanced process analytics• VTT´s other research services

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