Pesquisas em materiais polimricos: tendncias internacionais para o setor industrial

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  1. 1. 7o WORKSHOP INTERNACIONAL SENAI MATERIAIS30 de ogosto 2012; Cricima SC Brasil"Tendncias de Pesquisa, Desenvolvimento e Inovaodos Materiais para Aplicaes Industriais" Pesquisas em materiais polimricos:tendncias internacionaispara o setor industrialErich Meusel; Rdiger Strubl; Wolfgang Mller; Ralf-Peter Gottlber;Nicole Klose; Frances Stckner; Anne Bhm; Klaus HeinemannThringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V.07407 Rudolstadt - Schwarza; GERMANY; E-Mail: heinemann@titk.deThringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Prof. Dr. Klaus Heinemann
  2. 2. DispositionPolymer materials research: International highly topical trends for the industry sector TITK industrial polymeric materials research institute,in the Free State "Thuringia"; Germany Material design using native polymers, esp. Cellulosethe TITK Fibre reinforced materials for the lightweight constructionALCERU high tech Nano-composites polymer materials with uncommon properties Specialized additives aiming at "macromolecular engineering"Fibre reinforcement Reactive "lcps": Basic concept for lc- PEIANano- composites Selected results Functionalized Nano- layered silicates:PEIA- modified nanoclaysSpecialized additives antibacterial nanoclays- reactive lcpsAdditives enriched- PEIA-nanoclaysat filament surface: Conception basic idea- antibac- nanoclays Design and synthesis of the novel additives- additives enriched Filament properties first resultsat the surface Rsum and outlookPOLYTRONIC Functional polymer systems and "POLYTRONIC"Fig. 02 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V.Prof. Dr. Klaus Heinemann
  3. 3. The TITK 58 Years Industrial ResearchThringisches Institutfr Textil- undKunststoff- Forschung e.V. Chemical Research Plastics ResearchTextile andMaterialResearch Functional PolymerInnovationCompetence Quality Systems and for a progressive productive small and medium-sized industry physical Research Dr.-Ing. Ralf-Uwe Bauer Managing Director of the TITK reg. assoc.
  4. 4. TITK the Research Institute forPolymer Materials Innovation CompetenceQuality
  5. 5. ThuringianThuringian Institute and Plastics Research Rudolstadt/ Germany Institute for Textile for Plastics Research (TITK) Rudolstadt / Germany Department of Functional Polymers SystemsTechnology triangle Jena Rudolstadt Ilmenau Friedrich-Schiller University of Jena Erfurt Weimar Jena A4 B88 B85 A71A9Ilmenau B88 RudolstadtUniversity ofTechnologyIlmenau Saalfeld / ICE ThuringiaCenter for Micro- andNanotechnologyRudolstadt
  6. 6. TITK - NetworkTITK OMPGThuringian Institute for Textile andEast Thuringian Material Testing Comp.Plastics Research reg. assoc. for Textiles and PlasticsEmployee: 133 Employee: 44Member:89Budget:10 million EUROTurnover: 5 million EUROResearch & Development(100% subsidiary of TITK)regardingMaterials, Materials Testing andProcessing and Technologies Characterization Services 25,1 % 28 % 33 % 50 %34 %Shanghai LyocellAPFIBRE Technologiegesell- Rubitherm Chemical Fibre GmbHschaft ThringenCompoundEngineering Rudolstadt mbG & Co. KG GmbHDevelopment Co.,Ltd.Fig. 06 Thringisches Institut fr Textil- und Kunststoff-Forschung
  7. 7. Thringisches Institut frTextil- und Kunststoff- Forschung e.V. Ostthringische Materialprfgesellschaft m. b. H.Accredited Testing of PlasticsSERVICE Advisory Centre regarding Material Applications Analyses of Recycling Materials InvestigationsTESTINGS ANALYSES Thermical testings Identification of plastics Mechanical testings Optical testings Flammability testings Electrical testingsOMChemical AnalysesDamage analysesParticle andSurface analyses Rheological testingsPGCo- Benefactor of the endowed professorship Plastics technology at the "University of Technology Ilmenau"Fig. 07
  8. 8. TITK - Network Research & Development regarding Materials, Processing and Technologies East Thuringian Material Testing Company for Textiles and Plastics (100% subsidiary of TITK) Materials Testing and Characterization Services including: Production of applicators for the Cosmetic Industry by electrostatic coating using flock fibresFig. 08 Thringisches Institut fr Textil- und Kunststoff-Forschung
  9. 9. Thringisches Institut fr Textil- und Kunststoff-Forschung Strategic Research Orientation: Industrial UtilizationNative Polymers andTextile andChemical Research Material Research Functional Polymers Composite MaterialsStructural Polymers Plastics ProcessingFunctional PolymerPlastics Research Systems Research Research Services, providing the Expertise and Potentials of the TITK to the small and medium-sized companies for their own developments Portfolio Research and Development Services: Processes and Materials Materials Testing and Characterization Services Selling of Products and Materials resulting from previous Research andDevelopment Activities and produced in small scale production Selling of own Patents respectively Licences
  10. 10. Department: Native Polymers and Chemical ResearchDr. Frank Meister Head of the departmentField of Research: Structural and functional materials based on Native PolymersCompetences:- Characterization of polymers and polymer solutions- Shaping of native polymersinto monofilaments, multifilaments, fibres, films and beadsby means of dry -wet or wet techniques- Chemical modification of polysaccharides and proteinsas well as their shaping for technical applications- Technologies for production of ceramic fibres and foilsFig. 10 Thringisches Institut fr Textil- und Kunststoff-Forschung
  11. 11. 1. Native Polymers and Chemical Research ALCERU - products an Overview ALCERU duothermALCERU piezoThringisches Institutfr Textil- und ALCERU beadsKunststoff- Forschung e.V. 0.450.4Polymer/Solvent-System : Polystyrene/THF34 5 nm Pore surface/pore volume : 59 10 m3/cm3 0.35Water retention behaviour: 16 cm3/g Chemical 0.3PSD (volume) 0.25 Research 0.2 0.150.1 0.05 ALCERU ceramic 005 1015 2025 30 354045 Information: PSS GmbH MainzTransverse pore diameter [nm] Plastics Research ALCERU supersorb900800Destw asser700 0.9% NaCl-LsungTextile and 600knstl. BlutMaterial R %WV[ ]500400Research300 ALCERU200100 conductive ALCERU exchange0010 20304050 SAP-Gehalt [%] Functional Polymer Systems and physical Research REM micrograph of ALCERU-supersorb fibres+ Ag+ 2m Dr.-Ing. Ralf-Uwe Bauer Managing Director of the TITK reg. assoc. ALCERU antibacterial
  12. 12. "Cell SolutionTM clima" a high potential PCM micro-composite material Composition: a new textile micro-composite material with thermo regulating properties PCM (Phase Change Material) is directly and permanently embedded in the fibre cross-section via dry-jet-wet spinning process highest heat storage capacity (up to 40 Joules per gram of fibre)Yarn composition / Fibre characteristics- cellulose > 47 %- PCM component 30 - 40 % (absolute)- minerals about 7 %- humidity < 12 %- finishing agent < 2 %- fibre fineness 2.2 - 6.7 dtex (according to customers demands)- staple length 38 - 60 mm (according to customers demands)- tenacity > 16 cN/tex- fibre elongation > 10 %- typical phase change temperature* 28 - 35 CEffectivity: proved washing permanence up to 50 washing cycles at 60 C excellent textile processability and dyeable in all colour gradations at least 10 % of Cell SolutionTM clima fibres in blended yarn (cotton, lyocell, viscose, wool, polyamide, polyester, ...) or fabric are recommended outstanding wearing comfort and micro climate because of excellent skin temperature regulation in bed textiles & heat or cold protection clothesDr. Frank Meister, Head of DepartmentFig. 12
  13. 13. Permethrin - based Nanocomposite ALCERU-FiberRequirements: increasing of blocking effect regarding blood-sucking insects lower insecticide contamination of clothes wearerT- shirt made of yarnscontaining 7 % functional fibresEvaluation "Cell SolutionTM protection"of fibres and fabrics madefrom insect blocking fibresdemonstratethe functionalityeven after 50 washing cycles 3-Phenoxybenzyl(1RS)-cis,trans-3-(2,2-dichlorovinyl)-and their safety2,2-dimethylcyclopropanecarboxylateat typical usagePermethrinFig. 13Thringisches Institut fr Textil- und Kunststoff-Forschung
  14. 14. Flame- resistant melamine melt- blown fibre matsScheme of modified meltblown process (mini plant at TITK):MER melamine resin granulate Constructional CatalystIndustryCrosslinkingHot air>180C MeltblownTempering,fibre jet+FinishingConsolidation(if needed)Conveying screen typical value ranges: 10 m ~1m, 35 - 350 g/m,30 cm width (pilot plant) inherent flame resistance: LOI = 32 dont shrink, melt or drip when exposed to a flame excellent heat dimensional stability high thermal & acoustic insulation properties textile processability self- bonded web high filtration efficiency Excellent chemical resistance especiallyagainstalkali and organics; fair acid - resistantFig. 14 Thringisches Institut fr Textil- und Kunststoff-Forschung
  15. 15. 2. Textile and Material ResearchResearch Fields Fibre Reinforced Composites materials and their production technologies Technical Textiles textile composites, sandwich - structures (light- weight materials) and recycling as well as reutilization processes High Performance Fibres and Textile Fabrics Usage as reinforcing materials and other technical applications Materials Testing /CharacterizationDr. Renate Ltzkendorf, Head of DepartmentFig. 15
  16. 16. 2. Textile and Material ResearchFiber reinforced composites New developments:Composites reinforced with CARBON fibresComposites reinforced with ARAMIDE fibres"Long fibres reinforced granulates" developmentsand result in ARAMIDE - Recycling fibresThermoplastic Matrix fibres Long fibres reinforced granulatesMatrix materials: PP; PA 6; PA 6.6ARAMIDE - content: up to 70%Applications: - Compounding;- Injection mouldingIndustry: - Automobiles- TyresDr. Renate Ltzkendorf, Head of DepartmentFig. 16
  17. 17. 3. Plastics Research Dr. Stefan Reinemann head of the department Focus of Research ActivitiesThringisches Institut CompoundingInjectionfr Textil- und Development of Formulations, MouldingKunststoff- Forschung e.V. Processing technologies and Processing methods Plastics Research Characterization of the Material Behaviour of thermoplastic polymers with the main topics: Chemical- Nanocomposites: Carbon Nano Tubes (CNT) Research expanded graphiteFilms and Sheetslayered silicates Textile and - Compounds using el. conductive additives EM- Shielding Material- Synthetic / Natural / Glass Fibre reinforced Compounds Research - Fire - retardant modification and testing - in-situ-Modification of Polyesters / Polyamides Functional- Catalysis of Polyesters / Polyamides Polymer - Nanocapsules with core - shell architectures Systems and physical by means of DENDRITIC POLYMERS Research Material specific Plastics Recycling Dr.-Ing. Ralf-Uwe Bauer Conceptions, Processes, Products Managing Director Transfer Centre for Technologies of the TITK reg. assoc. of material specific Plastics Recycling Extrusion
  18. 18. 3. Department: Plastics Research Fibre reinforced Polypropylene using Synthetic fibres, e.g. PET or PAN Results using PAN fibres:- increase of the STRENGTH: up to 30%- enhancement of the STIFFNESS: up to 50%- improvement of the IMPACT TOUGTNESS:up to 500%"Falling-ball impact test" (- 30C)0% PAN10% PAN20% PAN30% PANDr. Stefan Reinemann, Head of DepartmentFig. 18
  19. 19. 2. Department: Plastics ResearchEffect of"PA 6 / PP - OMMT - Nanocomposite" BlendsFig. 19 Thringisches Institut fr Textil- und Kunststoff-Forschung e.V.
  20. 20. 3. Department: Plastics ResearchHeat accumulating and Heat storing polymer granulatesaccumulating process loaded pull - out process unloaded PCM containing Polymer Granulate Material: Melting temperatures of the PCMs used are determining the accumulating and the pull - out temperatures of the heat storage granul es,[e.g. (6 / 42 / 52 / 58 und 82) C] Applications as buffer store for: - Thermal Solar Collectors - Heat Pumps (cold and/or warm site) REM Foto: Einlagerung des Wrmespeicher-Paraffinsin der Polymermatrix - Solid - phase burning oven / oil or gas burner / air-conditioning systems, engine heatFig. 20 Thringisches Institut fr Textil- und Kunststoff-Forschung e.V.
  21. 21. Heat accumulating and Heat storing polymer granulatesReference and Demonstration apparatus at TITKStation III :Floor heating zone Heated area office floor:ca. 60 m Collector area:ca. 52 m2 20 Sunlight Collectors: (BUDERUS SKB4.0-w) Installed Solar power:26 31 KW Phase Change Temperature:42 C PCM - Granulate Mass: 1000 kg height of the granulate bed:4 cm Heat power Output: ca. 40 kW Floor surface temperature: ca. 30 C Fig. 1: Schematic Plan of the Solar Thermal Floor HeatingFig. 2: Schematic Layoutof the Floor21Fig. 21
  22. 22. TITK- department: Plastics Research Autoclave Technology Syntheses of POLYESTERS (PET, PTT, PBT and PEN) Modification of polyesters using Co-monomers "in-situ"- modification of polyesters using various additives Evaluation of catalyzer systems for polyester syntheses Equipment:2L- Autoclave 10L- Autoclave- overpressure up to 15 bar - overpressure up to 20 bar- polymer yield up to 1 kg- polymer yield up to 6 kg Syntheses of POLYAMIDES (PA 6, PA 6.6) Modification of polyamides using Co-monomers "in-situ"- modification of polyamides using additives Equipment:10L-Autoclave for (trans)esterification and polycondensation5L- Autoclave 10L- Autoclave (t < 320 C)- overpressure up to 20 bar - overpressure up to 25 bar- polymer yield up to 3 kg- polymer yield up to 5 kg New equipment for "up-scaling" of polymer syntheses,including Finisher to increase the melt viscosity (mbatch ~ 30 kg)Dr. Stefan Reinemann; head of the departmentFig. 22
  23. 23. Department: Functional Polymer Systems and Physical Research Head of the department: Prof. Dr. Klaus Heinemannconsists of two Research Teams:Synthetic Functional Polymer Materials and compositesOrganic Nano - Layers and layer systemsas well asMicro Structuring and materials patterning technologiesfor POLYMER ELECTRONIC (IC&M Technologies),MICROSYSTEM, MEDICINE and TRANSPORT Applic.Chemical and physico - chemical modification oftechnical High- Performance- and High- Tech polymersusing functional, migrating or reactive additives to thegeneration of specific surface or interface propertiesand/or special material functionalities,including their processing to films and filamentsfor the FIBRE and POLYMER PROCESSING INDUSTRIE
  24. 24. N NC CSynthesis ChemistryO_nLCP modified polyamide and polyester resins and fibres_ Flame - retardant polyamide and polyester resins and fibres_ Surface - modified polymer films and fibres_ reactive polymer blending and fibres thereof_ Polymer modification by reactive compounding using"chain extender" or "reactive modifier" and fibres thereof_ Permanent hydrophobic modification of polyamides & polyesters_ Permanent hydrophilic modification of polyamides & polyesters_ Fluorescent polyamide and polyester fibres_ Functional polymer systems for smart fibres and smart textiles_ Bi- component High temperature melt spinning technologywith velocities up to 6.000 m/min (LOY, POY,HOY, FOY)Fig. 24 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  25. 25. O O C C O O C C O OC COOCCO n OOO = 250 C m = 6,5 kg / h DZ = 200 / min+ (2n + 2) H2N PA 6COOH t = 2 min ZSK 25 Fa. Werner&Pfleiderer- ( 2 n + 2 ) H2O OO CCHOOC PA N N PA COOH CC OOC COOC CO nONNPA PACO OHCOOH Reaction of lc poly (esterimide anhydrides) with PA 6 Fig. 25 in molten state to form graft - block - copolyesterimides
  26. 26. Mode of action in polyamide fibresUV- or light PA 6 incompatible component stabilizer molecule(migration causing element)reactive lcpsPEIA &in reality:NanoclaysAntibac FORMATIONNanoclaysOF AAdditives CONCENTRATIONenrichedGRADIENT !at the surfaceconception may be expectedbasic ideaobjectives component with PA 6 affinitysyntheses (anchoring segment) PA 6 fibre surfaceprocessingresults Spontaneous migration of the stabilizer additives during the fibre forming processanalyses Enrichment of the stabilizer molecules nearby the boundary layer of PA fibrersumoutlookImmobilization of the complex additives molecule in the accomplished fibrethe TITK Improved light protection efficiency by accessibility of stabilizer molecules in the surface regionFig. 26Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V.Prof. Dr. Klaus Heinemann
  27. 27. Reactive Complex- forming agent s BiocidesApplication of a novel Silver Salt Complex in PA 6.6Reference250 ppm 750 ppm1500 ppm5000 ppmFig. 27 Thringisches InstitutInstitut frfr Textil- und Kunststoff-Forschung Thringisches fr Textil- und Kunststoff-ForschungThringisches Institut Textil- und Kunststoff-ForschungSteffi Sensfussund TeamDr. R. Strubl
  28. 28. Modular multifunctional apparatus for additive synthesesFig. 28 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  29. 29. Modular multifunctional apparatus for additive synthesesChemical syntheses in liquid media, also under explosion- protected conditions Batch- Volumes:10 Litre (stainless steel) and 16 Litre (titanium) Reaction temperatures: up to 200 Cup to 300 C Reaction pressures:up to 0,5 bar Reaction media:homogeneous and heterogeneous phases Isolation of products:vacuum distillation; evaporation; phase separation; Extraction;for: alkylations; acylations halogenations; nitrations; sulphonations; epoxidations esterifications; transesterifications; amidations; saponification Online-IR-Spectroscopy for reaction analysis und -optimization (7 bar) Calorimetry of reactions, also in case of increased pressure (100 bar)Compound separations by vacuum distillation up to 15 kg/h (offer of service)Chemical syntheses at Kilogram scale (customer order)Fig. 29 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  30. 30. Department of FUNCTIONAL POLYMER SYSTEMS Processing EquipmentFig. 30 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  31. 31. Micro twin- screw melt compounder & spinning device Technical Parameters:- Polymer melt temperatures: 350 C;- Melt volume Polymer mass: v = 5,5 cm3; m ~ 8 g !!!;- Screw speed:n = (1 360) min-1HAAKE MiniLab Thermo ELECTRON GmbH76227 KarlsruheFig. 31 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  32. 32. Micro melt spinning apparatusMicro extrusion system Minitruder (Fa. Randcastle Inc.; USA)- Polymer melt temperatures: max 430 C- throughputs:10 - 120 g/hor80 - 980 g/hFig. 32 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  33. 33. Bicomponent High temperature melt spinning device with winding speeds up to 6.000 m/min Bicomponent nozzleouterinnerannular gap (sheath) (core)Quelle: EMPA & Fa. FournFig. 33 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  34. 34. POLYTRONICFocus: Generation of polymer-based electronic system components Functional Polymer Systems: from Material to SystemTechnology developments in the direction of upscaling ofexplored microtechnologies of "polymer engineering" in favour of thescientific and technical prearrangement of the serial manufacturing of: Polymer- based field effect transistors and integrated circuits, Sensors, Actuators, Photovoltaic Cells und Modules as well as Modules by using substances with switchableelectrochromic, photochromic and thermochromic properties;for applications regardinginformation-, communication- and media technology, microelectronics,microsystems-, medical- and traffic technology, including"Reel-to-Reel"- Technologies for - coating and - micro structuringFig. 34 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Rdiger Strubl & Team
  35. 35. Department: Functional Polymer Systems I. Topic: Polymer Electronic ApplicationsSchematic View of a PFET (Polymer-Field-Effect-Transistor) on a flexible polymer film2 mmmetal or d: 100 - 3.000 nmGate electrodeconductingpolymer Insulator (d: 400 nm 1.000 nm(PANI,PEDOT:PSS)Semi conductorPoly(3-alkyl- (d: 5 nm 50 nm)thiophenes)metal, ITO or drainconductingpolymer source (PANI, 0,5 - 3 mm PEDOT:PSS)PET; PI; ABS; glass flexible polymer substrate d: 100 - 200 mFig. 35 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrdner & Team
  36. 36. Department: Functional Polymer Systems II. Topic: Flexible Polymer Photovoltaic Possible Applications: Solar cells on tents(esp. for aid organisations) Solar cells on textiles[esp. for military and sport textiles (GPS)] Solar cells on credit cards(credit cards real smart cards)Fig. 36 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V. Dr. Mario Schrdner & Team
  37. 37. II. Topic: Flexible Polymer Photovoltaic PPossible Applications:Portable PV-Consumer Moduleselectronics intelligent electronic packaging textilesModules oncurved surfacesBuilding IntegrationSmart cards 80 1 .9 23 4 56 70 89 * 0# (BIPV)Fig. 37 Thringisches Institut fr Textil- und Kunststoff-Forschung (TITK) e. V.Frau Dr. Steffi Sensfu & Team
  38. 38. department: Functional Polymer Systems "POLYTRONIC"I. Topic: II. Topic: Polymer Solar CellApplications:Polymer-Field-Effect-Transistors Schematic Drawing PFETIII. Topic:Micro- and Nanometre-thin Functional Layers by Reel - to - Reel Technology Coating Equipment "LBA 200"Fig. 38 Dr. Schrdner & Team
  39. 39. Reel to Reel coating equipment LBA 200 Antrag Lsungsmittel IR-Feld Beschich- tungsmittelT Trocknung-/ ErstarrungsstreckeCoronaAbwicklungAufwicklung SteuerungPC Rolle - zu - RolleParameters:Width of the substrate tape: 20 cmSpeed of the tape: 10 m/minCorona Activation:2.5 kWInfrared dryer: 3.4 kWHot air dryer:80 120 C Continuous wet coating usingdiluted polymer- solutions/ -dispersions by means of Reel- to- Reel TechnologyFig. 39Thringisches Institut fr Textil- und Kunststoff-Forschung Frau DP K. Schultheis; Dr. L. Blankenburg
  40. 40. Roll-to-Roll (R2R) Coating Technology processing flexible Polymer Solar Cells Spin coatingDoctor blading continuous coating R2RProcessing parameters R2RMaterials- Substrate: PET/ITO (175 m)- Baytron PH (~100 nm)- P3HT/PCBM (1:1) 1.2% in Chlorobenzene (~60 - 150 nm)Technology parameters- Corona pre- treatment: 200 W- Velocity of the band: 1 - 2 m/min 20- Width of the slot: 3 - 5 cmdark illuminated- Dosing rate: 1 - 5 ml/min 15- Circulating air drying: 80 C (Baytron)ISC:6.13 mA/cm210 VOC:618 mVcurrent [mA/cm ] 2 FF: 0.46Completing of the Cells - discontinuousAM1.5: 1.74 %5- Vapour deposition of the Al- electrode- Annealing: 5 min at 100C 0 -0,50 0,5 1Measuring conditions Cell characterisation-5- AM 1.5- Cell dimension: 5x5 mm -10bias [V]- environmental conditionsEfficiencies: Spincoating = 5,4 % R2R = 1,7 % 4,5 %Fig. 40 Thringisches Institut fr Textil- und Kunststoff-Forschung Frau DP K. Schultheis; Dr. L. Blankenburg