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  2. 2. CONTENT-• Introduction• Purposes• Period of drying• Classification of dryers• Special types of dryers• references
  3. 3. INTRODUCTION TO DRYING PROCESS Drying can be described by three processes operating simultaneously: 1. Energy transfer from an external source to the water or organic solvent  Direct or Indirect Heat Transfer 2. Phase transformation of water/solvent from a liquid- like state to a vapour state  Mass Transfer (solid characteristics) 3. Transfer vapour generated away from the API and out of the drying equipment
  4. 4.  Drying APIs is an important operation for the production of consistent, stable, free-flowing materials for formulation, packaging, storage and transport Particle attrition or agglomeration can result in major differences in particle size distribution (PSD), compressibility and flow characteristics Equipment selection Drying specifications
  5. 5.  Purpose: To reduce the moisture level of wet granules Why do it What are the What are the problems equipment To keep the residual Direct Heating Static Over drying (bone dry) moisture low enough Solids Bed Dryers (preferably as a range) to Excess fines prevent product Direct Heating Moving deterioration Solids Bed Dryers Possible fire hazard Ensure free flowing Fluid Bed Dryer properties Indirect Conduction Dryers
  6. 6. PERIODS OF DRYING •Warm up period :A-B •Constant Rate Period (B-C)  HT dependent •Falling rate period (C-D)  MT dependent
  7. 7. DRYERS IN THE PHARMA INDUSTRY Dryers can be classified according to:  Heat transferring methods  Direct: Fluidised, Tray, Spray, Rotary Dryers, etc..  Indirect: Cone, Tumble, Pan Dryers, etc…  Continuous/ Batch processing  Continuous: large quantities/small residence time  Batch: small quantities/ long residence time
  8. 8. TRAY DRYERS a batch tray dryeR consists of a stack of trays or several stacks of trays placed in a large insulated chamber in which hot air is circulated with appropriately designed fans and guide vanes.
  9. 9.  It is possible to convert the batch tray dryer into a continuous unit. Figure shows the so-called Turbo dryer, which consists of a stack of coaxial circular trays mounted on a single vertical shaft. The product layer fed onto the first shelf is leveled by a set of stationary blades, which scratch a series of grooves into the layer surface. The blades are staggered to ensure mixing of the material.
  10. 10. ROTARY DRYERS The cascading rotary dryer is a continuously operated direct contact dryer consisting of a slowly revolving cylindrical shell that is typically inclined to the horizontal a few degrees to aid the transportation of the wet feedstock which is introduced into the drum at the upper end and the dried product withdrawn at the lower end.
  11. 11.  VACCUM DRYERSFor drying of granular solids or slurries, vacuum dryers of various mechanical designs are available commercially. They are more expensive than atmospheric pressure dryers but are suited for heat-sensitive materials or when solvent recovery is required
  12. 12. FLUID-BED DRYERS (FLUIDIZED-BED DRYERS•Concept of fluidization•Gas velocity realizing the change fromstationary(fixed) bed into fluidized bed iscalled the critical fluidized velocityucritical.•When gas velocity is increased to theparticle free setting velocity u0 , theparticle will be carried over, u0 is called thecarried over velocity ucarried.ucritical<uoptimum<ucarried 7
  13. 13. •CHARACTERISTICS OF FLUID-BED to Dust CollectorDRYERS: ADVANTAGES:HIGH HEAT AND FeedMASS TRANSFER RATES; SIMPLE Hot Air to Dust Collector product discharge Distributo r PlateSTRUCTURES; LOW FABRICATING Feed to Dust Collector Dry product disch arg eCOSTS; CONVENIENT MAINTENANCE; Hot Air Dust Feed to Collector to Dust Collector Feed Hot AirHIGHER THERMAL EFFICIENCY THAN Distributo r Plate Feed Hot Dry product Air Distributo r Plate disch arg ePNEUMATIC CONVEYING DRYERS; Hot AirDistributo r Plate Dry product discDRYING TIME CAN BE CHANGED; Distributo r product disch arg e Dry PlateAPPLIED TO DRYING OF GRANULAR Dry product disch arg e Horizontally separatelyMATERIALS. fluidized compartments (Fig. 5-25) can get even•DISADVANTAGES: STRICT OPERATION drying and relatively lowAND CONTROL REQUIREMENTS; flow resistance.MULTI-SEPARATELY FLUIDIZEDCOMPARTMENTS(PLUG FLOWDRYERS) HAVE COMPLEX 8STRUCTURES AND GREAT FLOW
  14. 14. Feed (3)PNEUMATIC CONVEYING DRYERS Section Feed First First Section Second Section Feed Feed First Section Characteristics: Second Section Room for separating solids 1)Great First Section Section Second contacting area between Room for separating solids air Feed Cleaned air Feed Feed and solids;Higher heat air Feed Cleaned SecondRoom for sep Section First Section First separatin transfer and mass transfer Feed ExhaustSection Section Exhaust air First air First Feed for Section Room Cleaned air rates; Short drying Second Section Exhaust Section First Second Cleaned Section air air First Section Section Section Second Second Room for separatingforsolid Second Section sepa Room time(0.5~2s). Exhaust for separating air 2)Stable operation and fine Second Room for separating solidsRoomCleaned air Section Room for separating solids Feed product quality. Cleaned air Cleaned air air Exhaust RoomFirst Section for separating solids Cleaned Cleaned Exhaust air Exhaust air air air CleanedExhaust air air Second Section air Exhaust Exhaust air for separating solids Room 3)Applying to thermally sensitive and air Cleaned easily oxidized materials. Exhaust airDefects: Materials easily broken; great flow resistance; highdrying duct. (about 30m) 5
  15. 15. FREEZE DRYER Highly heat-sensitive solids, such as some certain biotechnological materials, pharmaceuticals and foods with high flavor content, may be freeze dried at a cost that is at least one order-of-magnitude higher than that of spray drying – itself not an inexpensive drying operation. Here, drying occurs below the triple point of the liquid by sublimation of the frozen moisture into vapor, which is then removed from the drying chamber by mechanical vacuum pumps or steam jet ejectors. Generally, freeze drying yields the highest quality product of any dehydration techniques
  16. 16. BASIC ISSUES FOR PHARMACEUTICAL FREEZE-DRYING 7.1.1 New Dosage forms of pharmaceutical drugs According to its development, pharmaceutical dosage form can be divided into the following generations:  The first generation : simple ointment, pill and powder for oral administration and external use.  The second generation: the tablets, injections, capsules and aerosols made by mechanical and automatic machines.  The third generation: slow-release or controlled-release dosage forms that form a new drug delivery system (DDS) .  The fourth generation:targeted dosage forms that form a targeted drug delivery system.  The fifth generation: the automatic release dosage forms inside the body when the patients have a serious illness. At present, the third and fourth generations of dosage forms are most concerned by scientists.
  17. 17.  In order to realize these new drug delivery system, many new techniques are developed in the formulation of dosage form, such as  solid dispersion,  inclusion,  emulsion,  liposomes,  microencapsulation.
  18. 18. 7.1.3 BASIC PROCESS OF BIOLOGICAL DRUGS FREEZE-DRYING The technical procedures of drug freeze-drying consist of four processes:  preparation and freezing,  primary drying (sublimation drying),  secondary drying (desorption drying)  package. The temperature, vacuum for each process have to be controlled precisely. The freeze-dried drugs are dry and porous solids.  They can be stored in room temperature or in refrigerator for a long time.
  19. 19.  1. Preparation and freezing of drugs  In order to form a stable porous structure after freeze drying, the concentration of drug solution must be a specific value.  Excipients should be added into the low dose thermal sensitive drugs (hormone, enzyme, vaccine) to reinforce the structure of freeze-dried products.  Lyoprotectant should be added into the biological protein-type drugs or slow-release drugs with bio-membrane to protect proteins from denaturation and the bio-membrane from damage.  The end temperature of pre-freezing must be lower than the glass transition temperature (Tg) or eutectic temperature (Te) of the drug solution.
  20. 20.  2. Primary drying (sublimation drying)  are performed at low temperature and vacuum.  The drying progresses gradually from the surface to the center of the products.  The pores or channels formed by the sublimation ice become the ways of vapor to escape.  The boundary between drying layer and frozen layer is known as the sublimation interface.  The temperature of the sublimation interface is a critical parameter to be controlled in primary drying process.  90% water in drugs is removed after primary drying.  In primary drying process, the temperature of frozen layer must be lower than Te or Tg’.  The temperature of dried layer must is lower than the collapse temperature (Tc).  The temperature of the heater in the drying chamber should be controlled strictly.
  21. 21.  3. Secondary drying (desorption drying)  purpose : to remove a portion of the bound water.  The moisture content of drugs is lower than 3% after secondary drying.  Because of large absorption energy, the product temperature in secondary drying must be increased high enough to remove the bound water, and on the other hand, this temperature cannot induce denaturation of proteins and deterioration of biological drugs.  The Tg of the products increases gradually with the decrement of water in secondary process.  So the drying temperature of the products can be increased gradually, but cannot be higher than Tg.
  22. 22.  4. Encapsulation process  When the secondary drying process is complete, plugging system in the chamber is used directly to plug the vials in order to prevent the freeze dried drugs from oxidation and water absorption.  The encapsulation can also be completed after filling nitrogen gas into the chamber.
  23. 23. 7.1.4 CHARACTERISTICS OF FREEZE-DRYINGTECHNOLOGY FOR DRUGS characteristics of freeze-drying technology for drugs are  can prevent the active components in from denaturation or loss of biological activity.  can protect the components in drugs from oxidation.  can greatly reduce the loss of volatile components in drugs.  can inhibit the growth of microorganism and the activity of enzyme in drugs.
  24. 24.  Freeze dried drugs will maintain the original structure. Freeze dried drugs have good rehydration property. Freeze dried drugs can be stored at room temperature for a long time The initial cost of freeze-drying equipment is larger. Freeze drying is a time and energy consuming process. It is very difficult to control the parameters at optimum level.
  25. 25. 7.1.5 CRITICAL PROBLEMS OF FREEZE-DRYING INDRUGS  1. Temperature Control and identification of drying procedures  Frozen drugs will melt, collapse or crimple if the temperature is higher than the optimum temperature.  if the temperature is too low, refrigeration load will causing excessive energy consumption and the sublimation rate will be decreased greatly
  26. 26.  2. Cooling Rate in freezing process  freezing process determines the drying rate and the quality of freeze-dried product.  The optimum cooling rates vary with different biological agents.For instance,  slow freezing is usually beneficial to protein polypeptide-type drugs.  Fast freezing is usually beneficial to the virus and vaccine.
  27. 27.  3. Types and concentration of lyoprotectant  The molecular structure of the active components is different for different biological agents.  The types and concentration of lyoprotectants required in freeze drying are also different.  Up to now, there is not a universal lyoprotectant applied to all of the biological agents.
  29. 29. DRUM DRYERS In drum dryers, slurries or pasty feedstocks are dried on the surface of a slowly rotating steam-heated drum. A thin film of the paste is applied on the surface in various ways. The dried film is doctored off once it is dry and collected as flakes (rather than powder).
  30. 30. BAND DRYER For relatively free-flowing granules and extrudates that may undergo mechanical damage if they are dispersed, band dryers are a good option. It is essentially a conveyor dryer wherein the band is a perforated band over which the bed of drying solids rests. Drying air at rather low velocities flows upwards through the band to accomplish drying.
  31. 31. TUNNEL DRYER In this simple dryer concept, cabinets, trucks or trolleys containing the material to be dried are transported at an appropriate speed through a long insulated chamber (or tunnel) while hot drying gas is made to flow in concurrent, countercurrent, cross-flow or mixed flow fashion. In the concurrent mode, the hottest and driest air meets the wetted material and hence results in high initial drying rates but with relatively low product temperature (wet-bulb temperature if surface moisture is present).
  32. 32. MICROWAVE (MW) AND RADIO FREQUENCY (RF)DRYING Unlike conduction, convection or radiation, dielectric heating heats a material containing a polar compound volumetrically, i.e., thermal energy supplied at the surface does not have to be conducted into the interior, as limited by Fouriers law of heatconduction. This type of heating provides the following advantages: · Enhanced diffusion of heat and mass · Development of internal pressure gradients which enhance drying rates · Increased drying rates without increasing surface temperatures · Better product quality
  34. 34. Thanks