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From an idea to the final product

Pilot plants

for bio and process technology


BUILDING PA R T N E R S H I P THROUGH INNOVATIONS V T T ’ s ser vices VTT’s services cover all key stages of the customer’s innovation process. Our aim is to increase the competitiveness of our customers’ businesses, promote the creation of new business, and improve and speed up the impact of R&D. We offer our customers access to our cross-disciplinary technological and business expertise, unique research infrastructure, and comprehensive partnership networks. Customized solutions are created in close cooperation with the customer. In the following pages you can find out how our Pilot services could enhance your competitiveness. Contact us for your tailored solution.

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Pilot plants for bio and process technology

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Process chemistry pilot plants

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Fermentation and downstream processing

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Food pilot plants

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Plastics processing pilots

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Editorial: Mika Härkönen, VTT Graphic design: Sari Halme, VTT Photos: VTT, Tekes, iStockphoto, Shutterstock This review is printed on Galerie Art Silk printing paper, which has been granted the environmental emblem of the Nordic countries. Printed in Edita Prima Ltd 2012

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Pilot plants

for bio and process technology Pilot it with VTT

WE WELCOME NEW CHALLENGES

The Pilot Plant Services at VTT assist the bioprocess, chemical, energy, forest, food and beverage industries to develop new processes and products, and predict scale-up effects. Pilot trials help to minimise risks and costs on the way from the laboratory to industrial production. We can help our customers with versatile product and process development tasks including custom manufacturing services provided by our highly skilled, experienced and customer-oriented personnel. We can provide a comprehensive scale-up service for small and large companies by combining piloting with VTT expertise in chemistry, biotechnology, analytics and application testing. VTT also provides process feasibility and sustainability assessments. We serve many types of customers, from large international food or chemical companies to small local biotechnology startup enterprises. Our pilot plants are located in Otaniemi and Rajamäki, both close to Helsinki, the capital of Finland.

VTT is your partner in developing your business. VTT is an impartial expert organisation that carries out technical and techno-economic research and development work. We also offer information services. VTT is a contract research organization involved in many international assignments. With its 3,200 employees, VTT provides a wide range of technology and applied research services for its clients, private companies, institutions and the public sector.

Customer need

Chemical reactions

WE CAN HELP WHEN • a hypothesis needs to be tested • a process needs to be scaled up or optimised • empirical production data is required for the design of a new plant or product • you need manufacturing services for your products • you don’t have the staff or equipment to do it all yourself.

Fermentations

Know-how

Experts

Food processing

Raw materials

Plastic processing

Equipment

Product recovery Characterisation

Products

Scale-up understanding

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Process chemistry pilot plants VTT´s process chemistry pilot plants have excellent facilities for rapid and efficient product and process development. We offer a unique combination of relatively large pilot scale multi-purpose reactors and versatile downstream processing units. SCALE-UP WITH VTT A special feature of our process chemistry pilots is relatively large-sized pilot plant equipment: multi-purpose reactors up to 2 m3 integrated with suitable downstream processing units. Therefore our pilot plants offer the possibility for relatively large scale pilot tests and custom manufacturing services e.g. for emerging SME companies. We have pilot facilities located in Rajamäki and Otaniemi, both near Helsinki. The total pilot hall area is 1200 m2, of which 300 m2 is ATEX-classified for handling of flammable chemicals. Customer personnel can participate in the test runs, and some of our equipment can be leased out for tests at other locations. Health, safety and environmental issues are an integral part of our daily work. Our customers are typically from chemical, biotechnology, forest and pharmaceutical industries. This means that very versatile tasks can be performed at

CHEMICAL pilot plant facilities Reactors • Two multi-purpose reactor systems: 60 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...+280 °C, pressure range: 10 mbar…60 bar • Reactors for viscous and corrosive materials 4

our pilot plants. Fractionation and chemistry of biomass-based materials and chemicals has been a focus area already for more than 15 years.

Multi- purpose reactor systems and versatile down stream processing VTT’s two multi-purpose reactor systems combined with versatile down stream processing units provide excellent possibilities for several industrial applications. We can perform tasks from biomass fractionations to challenging synthesis of fine chemicals.

Main capabilities • Multi-purpose reactors: steel and glass-lined pilot reactors having capacities between 60 and 1800 dm3 for chemical synthesis, polymerisations, distillations, extractions etc. Bench-scale reactors are also available.

• Drais/Lödige All-in-one-reactors: 5, 100, 130 and 250 dm3 (reaction, distillation, drying, granulation, dispersion), 10 mbar…25 bar, • Tube reactor • ATEX-classified Distillation, evaporation and drying • Conventional and vacuum distillation in reactor systems and separate distillers • Falling film evaporators (water 50 dm3/h, suitable also for organic solvents)

• Special reactors: for viscous and heterogeneous materials, dry and high consistency processing, biomass treatment and polymerisations, reaction calorimeter. • ATEX-classified facilities: handling of flammable substances. • Liquid-solid separations: separators, centrifuges and various filters. • Membrane filtrations: large pilot scale membrane filter units up to 40 m2 for controlled purifications. • Drying or concentration of slurries and solutions with vacuum contact and spray dryers. • Evaporations and distillations: falling film evaporators, distillation equipment, solvent recovery.

• Distillation unit (packed columns, vacuum,adjustable reflux ratio) • Vacuum contact dryers and evaporators Drais/Lödige 5, 100, 130 and 250 dm3 • Spray dryer, Niro P-6.3, 30-50 kg water/h • Fixed bed dryer (0.8 m3 ) • Rotavapor evaporator, 20 dm3, ATEX-classified


Examples of recent R&D activities • Pilot scale reactions: esterifications, etherifications, condensation and radical polymerisation, oxidation, chemical and enzymatic hydrolysis. • Chemical modifications of natural polymers, e.g. starch, hemicelluloses and cellulose fibres. • Formulation of products from chemically modified polysaccharides, e.g. adhesives, dispersions, pigments and bioplastics. • Recovery of valuable components from forest biomass followed by necessary purification, concentration and drying steps. For example, extraction of hemicellulose from pulp followed by membrane filtration purification and concentration or drying of the product. • Separation and recovery of the valuable components from microbial cells after fermentation. • High consistency processing and reactions. For example, pilot scale test runs to develop dry modification processes for starch. • Polymer production by radical, inonic and condensation polymerisations. • Utilising vacuum contact and spray dryers in drying of many types of materials. In addition, the contact dryers can be used for reactions, evaporations, compacting and granulation of materials, mixing, dispergation and coating.

Solid handling • 3-phase separator (feed max 5 m3/h), ATEX-classified (suitable also for flammable liquids) • 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) • Wet and dry mills

• In-line mixers (Silverson 425LS, Ytron Z60) • Materials AISI 316 Other process possibilities • Reaction calorimeter with NIR probe (Mettler Toledo RC1W, 100 bar) • Membrane cross-flow filtration units (up to 40 m2 ). Membrane types: tube, hollow fiber, spiral and plate. • VTT’s other research service

Additional informatION Pertti Tiitola Senior Specialist Pilot operations Tel. +358 40 502 6328 pertti.tiitola@vtt.fi Mika Härkönen Team Leader Pilot operations Tel. +358 40 083 9577 mika.harkonen@vtt.fi

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Fermentation and downstream processing VTT has comprehensive facilities for biotechnical process development. Our pilot hall has equipment for fermentation and downstream processing ranging from a scale of less than 1 litre up to 1,200 litres pilot scale and including a total of almost 50 bioreactors. Together with our competence in molecular biology and microbial physiology, we offer process development from the level of strain improvement to pilot scale technological production. For some of our customers, our pilot scale is in fact their production scale and we can thus offer routine contract production of materials.

Flexibility is an important feature in the Biotechnology pilot plant. Our processes have very varied aims and also requirements, which means that both the equipment and the operating personnel must be able to address a wide range of issues. Examples of processes operated in laboratory and pilot scale in recent years include: • Enzyme production for applications in the wood-, textile- and food processing industries, mainly but not only using the fungal host Trichoderma reesei. • Products for molecular biology research. • Plant and mammalian protein production in the yeast Pichia pastoris.

• Production of antibodies for diagnostic and other applications in E. coli in high cell density cultivation. • Active pharmaceutical ingredients for novel medicinal drugs, mainly using filamentous Streptomyces bacteria. • Production of cosmetics ingredients in plant cells in standard fermenters of up to 300 litres capacity. • Biofuel production including lipid compounds (biodiesel) and bioethanol using both yeast and filamentous fungi and also photosynthetic algae. • Continuous pilot scale bioethanol and biogas production from cellulosic materials via enzymatic hydrolysis and yeast fermentation.

Our downstream processing options include: • Cell separation by continuous separation and both vacuum drum and pressure filtration. • Product “polishing” by microfiltration to remove all process microbes. • Cell disruption by high pressure homogenization (600 bar) for release of intracellular products. • Protein concentration by tubular and plate-and-frame ultrafiltration. • Freeze-drying of e.g. cell- or protein concentrates (maximum capacity cf. 20 kg per run).

FERMENTER CAPACITY

PILOT FERMENTERS

• Open system (non-aseptic, non-

Three pilot fermenters (all from New LABORATORY FERMENTERS

Brunswick Scientific, USA)

Quoted volumes are maximum

• IF 40, working volume 28 dm3

working volumes.

• IF 400, working volume 300 dm3 • BioFlo PRO, working volume 1200 dm3

Autoclavable fermenters • 15 x 0.2 dm3 (local-made, prototype) • 6 x 0.5 dm3 (Infors, Switzerland) • 12 x 1.0 dm3 (Sartorius (Germany)

DOWNSTREAM PROCESSING EQUIPMENT Industrial technology in a research

Biostat Q+)

environment

• 2 x 2 dm3 (Sartorius Biostat B)

contained) • Suitable for separating e.g. fungal culture broths • Capacity 200-400 dm3/h depending on filtration qualities of the culture • Efficient clarification of most mycelial cultures CONTINUOUS CENTRIFUGATION • Alfa Laval separator, type BPTX 205SGD-30CDP • Capacity ca. 100-350 dm3/h ,

VACUUM DRUM FILTRATION

In situ-sterilizable fermenters • 6 x Sartorius CT-DCU 3 (4 x 2 dm , 3

• Larox (Finland, now Outotec) pilot scale drum filtration unit

2 x 5 dm3 ) • 2 x 7 dm3 (New Brunswick Scientific

• Precoat (filter aid) or belt filtration, filtering surface area 1 m2

(USA) Bioflo IV) • 2 x Sartorius C-DCU (10 & 20 dm ) 3

• Similar to corresponding industrial equipment

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10000 x g • Similar to corresponding industrial equipment • Closed system (contained, “almost aseptic”) • Suitable for yeast and bacterial cultures


Other operations, e.g. various extraction procedures, vacuum evaporation etc. are also available at other pilot facilities within VTT. In addition, protein purification by versatile chromatographic means is available in-house.

The pilot services at VTT assist the bioprocess, energy, forest and food and beverage industries in the development of new processes and products. Tests in pilot scale can be used to evaluate process concepts before scale-up into

CELL DISRUPTION

Plate and frame modules

• High-pressure homogeniser (Rannie,

• Millipore (France) Pellicon equipment,

Denmark), feed rate 50-60 dm3/h , max pressure 700 bar, mainly for bacteria and yeasts

  ULTRAFILTRATION Tubular modules • PCI (UK) membrane modules, 4 x 2.6 m2 • Identical to corresponding industrial equipment (higher process volumes → more tubes)

modules á 2 m2 • Identical to industrial equipment (higher process volumes → more units) • Cut-off 10 kDa for protein

full scale industrial production, which always involves huge investment costs. Information obtained in pilot scale can be of immense value prior to final decisionmaking.

Additional informatION Jouni Ahtinen Key Account Manager Tel. +358 50 353 1145 jouni.ahtinen@vtt.fi

concentration (4 modules; other cut-off units also obtainable) • Cut-off 1000 kDa D for microfiltration (4 modules) • Working pressure <1.0 bar, circulation

Michael Bailey Senior Scientist Tel. +358 50 516 0720 michael.bailey@vtt.fi

<50 dm3/min

• For concentration of proteins • Nominal cut-off 25 kDa, actual cut-off apparently lower • Working pressure >5 bar, circulation >50 dm3/min • Pressure-drop protection for unsupervised operation

FREEZE DRYING • Christ Epsilon 2-25 DS lyophilizer • Water removal from almost anything • Capacity 15-20 dm3 in open trays (non-aseptic) • Capacity 2-10 dm3 in sterilized vials

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Food pilot plants VTT offers process and product development services for food and beverage infustry in a pilot scale. With our long-term research experience and development know-how we can offer new solutions for ingredient production and design of value added products. Let our experts help you to minimise risks and costs on the way from laboratory to industrial production

VTT Food pilots offer experienced personnel and high quality equipment to carry out process and product development in pilot scale or to perform proof of concept trials with new product ideas. Our pilot plant also enables small-scale production for feasibility and consumer studies. Customer personnel can participate in the processing trials. Production facilities are strictly food grade and the products can be used for clinical, sensory or consumer evaluation.

We can provide full service with a comprehensive set of analytical tools to characterize the process and the product. In addition, products can be subjected to sensory profiling by a certified sensory panel. Pilot services can be accompanied with other research services such as literature reviews, development of new product concepts, identification of potential health effects and assessment of sustainability. Our broad network of industrial and scientific partners is available for complementary work. VTT can also take responsibility of arranging further product characterization, for example through clinical trials.

Grinding and fractioning

Thermo-mechanical processing

• Fine impact milling (pin discs and swing beater with grinding track or sieves): ca. 5–10 kg/h • Flaking: ca. 10–30 kg/h • Air classification: ca. 1–5 kg/h, max. 15,000 rpm rotor speed • Air-jet sieving ca. 10–100 g/h

• Twin-screw extrusion: ca. 1–10 kg/h • Pre-conditioning: ca. 4–6 kg/batch • High-pressure processing: ca. 50–100 g/batch, max 10,000 bar • Vessels for processing and fermentation of high consistency solutions: 1–10 dm3

Drying • Lyophilisation (freeze-drying): max. 20 kg frozen sample/batch • Fluidised bed drying: 3–10 kg/batch • Spray drying: 0.5–6 kg/h

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Examples of recent R&D activities • Production of healthy and tasty food ingredients by - microbes and enzymes - dry-fractionation • Efficient utilization of nutritious berry and cereal fractions in foods • Value added & affordable food products from plant-based sidestreams, such as cereal brans, brewers’ spent grains and press cakes from berries and rape seed • Starter cultures and probiotic bacteria in baking and beverages

Beverage pilot • Our malting and brewing facilities cover the complete barley-to-beer chain. In addition we have expertise and equipment for production of other alcoholic and non-alcoholic beverages.

Malting • Micro-malting units: 0.1–8 kg/batch • Pilot malting unit: 50 kg/batch

Brewing, extraction and fermentation • Wet and dry milling • Brewhouse: 10 and 100 dm3


VTT is actively developing new food solutions in a NUTRITECH programme (www.nutritech.fi) aiming at new concepts for promotion of consumer health and well-being. Pilot for food and ingredient production The pilot hall was renovated in 2009 following high hygienic standards. We have equipments for particle size reduction and separation of components by dry fractionation technologies. In addition, we provide different kinds of thermo-mechanical processes and drying operations.

• Mash filter and lauter tun for wort separation • Continuous fermentation by immobilized yeast • Regular fermentation in 2, 10 and 50 dm3 tall tubes • Sheet filters • Bottling

Pilot bakery • We are dedicated to development and small-scale production of novel bakery products, especially sourdough, high-fibre and/or wholegrain baking.

Baking

Additional informatION

• Screening and optimization of ingredients and baking processes • Analysis methods for predicting baking quality • Development of health promoting bakery products • Prolonged shelf-life of bakery products • Frozen dough technology • Enzyme applications • Sourdough applications • New product concepts, from innovation to implementation

Juhani Sibakov Research Scientist Tel. +358 40 536 3428 juhani.sibakov@vtt.fi Annika Wilhelmson Key Account Manager Tel. +358 44 555 7913 annika.wilhelmson@vtt.fi Mirja Mokkila Key Account Manager Tel. +358 40 525 7423 mirja.mokkila@vtt.fi

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Plastics processing pilots We are surrounded by plastics - there is virtually no consumer or industrial product without a plastic component. The VTT plastic processing pilot located in Tampere offers state-of-the-art tools to develop and scale-up new material solutions through thermoplastic processing and converting.

VTT is well-equipped with equipment for production of thermoplastic (melt processable) composite materials in the range of a few grams to pilot scale with techniques such as compounding, extrusion coating and profile extrusion, blow moulding, micropelletising, injection and compression moulding. The equipment and the processes are routinely modified for the needs of changing material combinations which are literally unlimited in number. The plastic processing and converting services can be complemented with high level material property testing and characterisation as well as versatile tools for material pre- and posttreatments.

What makes VTT’s capacity truly unique is the possibility for modification and synthesis of materials at the monomer stage, followed by polymerisation and versatile melt processing techniques including composite compounding and combination with other processing such as paper production. The whole chain from material production to modification and finally to application is controlled and can be modified according to customer needs. VTT has gained special competence in the areas of thermoplastic biocomposites and polymer nanocomposites. More recently plastic foaming has become one of our focus areas, supported by acquisition of two new equipment for physical foaming of materials both in laboratory and pilot scale.

PROCESSING FACILITIES

Injection moulding • ThermoElectron Mini-Injection moulding machine with moulds for e.g. tensile, impact, DMA specimen • Engel ES 200/50 HL with 50 tons clamping force, 25 mm screw and instrumented mould having interchangeable inserts • Demag Ergotech 100/420-120 EL Exis S with 100 tons clamping force, 22 mm screw, maximum injection speed 1000 mm/s

Compounding • ThermoHaake Mini-compounder • Several co-rotating 25 mm twinscrew extruders with L/D rations from 25 to 48 • Berstorff High speed compounder • 2 Brabender Plasticorders for batch and laboratory scale compounding with scCO2 feed for foaming and a Clean room option

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BIOCOMPOSITES The demand for renewable plastic materials is on steady growth. The price of plastics of non-renewable origin may be reduced with a low cost bio-based additives such as bark, sawdust or other side-stream materials. With proper composite design, these low cost, partially fibrous additives can also be expected to improve the properties of the plastics. A more ambitious target is the production of entirely bio-based material with technical properties similar to those of modern engineering plastics, even those with reinforcement. Ultimately, transparent materials with mechanical properties at the level of steel may be expected by a combination of nanoscale cellulose particles with the right resin – both with 100% bio-based content.

Extrusion • Tandem extrusion. 300 mm wide sheet preform, 3-layer film with N2-rinsing possibility for film and extrusion coating. Capacity for physical expansion of the core layer with supercritical liquids. • Mini-extrusion facility for small scale screening • Blown film extrusion • Extruder with 100 mm and 120 mm wide sheets preform and roundstrip with 4 screw geometries with different compression and a clean room possibility


Natural materials are a logical choice for reinforcement of bioplastics: the compatibility is usually better, the composition remains completely renewable and recycling by biodegradation or incineration causes no problems . These additives can be incorporated in the composite structure by melt compounding, using powerful mixing technologies to disperse the additives in the polymer melt. For good dispersion and distribution, the compatibility of the additives with the host polymers needs to be good. This can be ensured either by selection of the materials or by modification of the additive surface to create physical or chemical linkages between the two constituents. The world-class biocomposite experience of VTT has been accumulated and

tested in 20+ cooperative and contract research projects over 15 years.

Post processing facilities • MD-stretching unit • Biaxial laboratory stretcher Brückner

Coatings and surface treatments • AC Corona treatment unit • Atmospheric plasma treatment unit • Atmospheric plasma deposition unit

Milling and fractionation • Hosakawa Alpine Separating mill 100 g – 30 kg/h, Particle size 0.5 - 10 μm, Powder grading. • Hosokawa Alpine AHM-90 Pearl Mill with several pearl sets • Several Ball mills • Gala Micro-pelletiser for production of round 0.2-1 mm pellets for e.g. rotation moulding

POLYMER NANOCOMPOSITES Polymers compounded, milled or otherwise mixed with nano-metric size organic or inorganic filler materials enhance the performance of traditional plastic materials. With expertise and careful planning these polymeric materials can reach a new desired combination of properties due to the tailored interaction of the individual material components at the nanolevel. The polymer nanocomposites experience has been accumulated and tested in numerous cooperative and contract research projects during the past decade.

Technical approaches for new polymer nanocomposites • Highly conductive compounds, electrical and thermal conductivity for energy applications • Dielectric compounds for electrical applications • Gas and vapour barriers • Optimization of the overall performance profile of traditionally highly filled plastics, e.g. fire retardance, UV-resistance and/or mechanical properties

Additional informatION Outi Härkki Key Account Manager, Team Leader Functional plastics Tel. +358 40 164 7647 outi.harkki@vtt.fi

TESTING FACILITIES • Mechanical testing • Material properties • Microscopy and particle size analysis • Spectroscopy

Kalle Nättinen Principal Scientist, Team Leader Biomaterials and processing Tel. +358 40 534 2974 kalle.nattinen@vtt.fi

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VTT Technical Research Centre of Finland is the largest multitechnological applied research organisation in Northern Europe. VTT provides high-end technology solutions and innovation services. From its wide knowledge base, VTT can combine different technologies, create new innovations and a substantial range of world class technologies and applied research services thus improving its clientsâ&#x20AC;&#x2122; competitiveness and competence. Through its international scientific and technology network, VTT can produce information, upgrade technology knowledge, create business intelligence and value added to its stakeholders. VTT is a non-profit-making research organisation.

VTT TECHNICAL RESEARCH CENTRE OF FINLAND Tekniikantie 4 A, Espoo P.O. Box 1000, FI-02044 VTT, Finland Tel. +358 20 722 111, Fax +358 20 722 7001

www.vtt.fi


VTT pilot plants