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Drum drier
- liquid is applied to the surface of the drum and spread FREEZE DRYING/ LYOPHILIZATION
to a film - dry extremely heat-sensitive materials
- simplest method is where the drum dips into a feed pan - allows drying w/o excessive damage of proteins, blood
- rate is controlled by the speed of rotation of the drum products and microorganisms
and temp - initial liquid is frozen, pressure above frozen state
- drum can be heated by steam or warm water reduced (pressure below triple point), water removed by
- product is scraped by the means of a doctor knife sublimation (liquid-solid-vapour; all under 0 C)
- for starch products, ferrous salts, suspensions of kaolin, - triple point- all three phases coexist (610 Pa, 0.0075 C)
zinc oxide - for biological productsantibiotics, blood, vaccines,
Advantages: enzyme preparations, microbiological cultures
a) Rapid drying
b) Equipment is compact Problems:
c) Heating time is short (few seconds) a) Must be within -10 to -30C
d) Drum in a vacuum jacket (temp is reduced) b) Sublimation only occurs at frozen surface and
e) Product is in flake form slow process
Disadvantages: c) At low pressure, large volumes of water vapour
a) Operating conditions are critical are produced which must be rapidly removed to
b) Impose careful control on feed rate, film prevent the pressure rising above the triple point
thickness, speed of drum rotation and drum pressure
temperature d) Dry material often needs to be sterile
Advantages:
Spray drier a) Drying at very low temperatures- enzyme action
- large surface area for heat and mass transfer inhibited, chemical decomposition by hydrolysis is
- atomizing the liquid to small droplets minimized
- drying chamber resembles a cyclone- good air b) Product is light and porous
circulation, facilitates heat, encourages separation of c) Porous form is soluble
dried particles from air d) No concentration of the solution prior to drying
- jet atomizers easily blocked by rapid evaporation and e) Oxidation is minimized
deposition of solid on the nozzle and droplet size is likely Disadvantages:
to vary a) Porosity, ready solubility and complete dryness=
- rotary atomizer has the advantage of being equally hygroscopic product
effective with solutions or suspensions of solid and can b) Very slow process, expensive
operate efficiently at various feed rates
- rotates the drying droplets around the chamber to Stages of freeze drying process:
increase residence time and drying time Freezing stage
- filter the air and to heat it indirectly by heat - frozen before application of vacuum to avoid frothing
exchanger i) Shell freezing- fairly large volumes (blood products)
- uniform in appearance, easily recognizable - horizontally
- particle shape is hollow sphere sometimes with a small -slow and large crystals form= damage
hole blood cells and reduce viability of microbial
- any substance in solution or in suspension cultures
- most useful for thermolabile materials - vertical spin freezing
- for citric acid, sodium phosphate gelatine, starch, - solution supercools and freezes rapidly,
barium sulfate, calcium phosphate, powdered antibiotic formation of small ice crystals
formulations for reconstitution to syrup, dry powder ii) Centrifugal evaporative freezing (ampoules) - prevents
inhalers foaming
Advantages:
a) Millions of small droplets= large surface area for Vacuum application stage
heat and mass transfer= very rapid evaporation - drop the pressure below the triple point and remove the
(overall, few seconds) large volumes of low pressure vapour formed
b) Droplets do not attain high temp. Particles kept
cool by evaporative cooling Sublimation stage
c) High bulk density= rapid dissolution (large surface i) Primary drying- reduce moisture content of a freeze-
area) dried solid to 0.5%
d) Uniform and controllable particle size ii) Heat transfer- insufficient, longer process; excess heat-
e) Excellent flow and compaction prop for tablet melting
manufacture - added heat but no significant increase in
f) Low labour costs temperature
- prefrozen bottles- blood, shelf- frozen materials
Disadvantages: shelf, ampoulescentrifuge head
a) Equipment is very bulky and expensive iii) Vapour removal- to avoid pressure rise that stops
b) Overall thermal efficiency is low (air must be hot sublimation
when it leaves the drier to avoid condensation)
egramoran
- use efficient vacuum pumps (small scaletwo- Influence of Process Factors on Solute Migration
stage rotary pumps; large scaleejector pumps) Drying method
- absorb vapour (small scaledesiccant like - intergranular migration- whenever temperature gradient
phosphoruus pentoxide, cooled with solid carbon is present (convective drying)
dioxide; large scalemechanically refrigerated - microwave radiationminimizes solute migration
condensers) - methods that keep granules in motionabolish
iv) Rate of drying very slow intergranular migration (intragranular may still occur;
fluidized bed)
Secondary drying - vacuum tumblingreduce migration
- removal or residual moisture at the end of primary
drying Initial moisture content
- raising the temperature to 50-60 C - greater moisture content= greater moisture movement
egramoran