BTE3480 (Separation Processes for Biochemical Products)

Lecture Outline
Todays lecture will cover:
1. Drying principles: a. Water in solids & gases; b. Heat & mass transfer. 2. Dryers description & operations: a. Vacuum-shelf dryer; b. Rotary dryer; c. Spray dryer; b. Freeze dryer.

Heat & Mass Transfer During Drying:

Fundamental processes during drying

Transfer of heat to evaporate liquid.

Heat

Transfer of mass as a liquid or vapor within the solid and as a vapor from the surface of the solid.

Wet solid

Heat Transfer: The principal heat transfer mechanisms: 1. Conduction from a hot surface contacting the material; 2. Convection from a gas that contacts the material; 3. Radiation from a hot gas or hot surface; 4. Microwave heating that generate heat within the wet material. Conductive drying: heat is supplied through the surface of the dryer and transferred by conduction to the solids being dried. Fouriers law dT q = - k ----dy
Heat flux (flow rate of heat per unit area) Direction of heat flow Thermal conductivity of the solid Temperature

Convective drying: heat is transferred from a moving gas phase to a solid phase to be used for drying.
Gas bulk phase temperature

Q = h A (T Ts)
Rate of heat flow into solid Heat transfer coefficient Surface area through which heat flows Temperature at the solid surface

Mass Transfer: The drying rate has been found to show certain phases:
During drying, water at the surface is the first to evaporate. B to C water move to the surface rapid enough that the surface remains saturated the drying rate is constant. C to D internal movement of water not fast enough to keep the surface saturated the drying rate falls. Asymptotically approaches the EMC.

Critical Moisture Content (CMC)

Equilibrium Moisture Content (EMC)

The drying phases can also be shown if the moisture content is plotted against time:
Constant-rate period linear rate
Falling-rate period rate of moisture loss decreases
CMC

EMC

2. Dryers Description & Operation

Factors to consider in choosing the right dryer: 1. Heat sensitivity of the material being dried; 2. Physical characteristic of the material; 3. The necessity for asepsis; 4. Nature of the liquid to be removed; 5. Scale of the operation; 6. Available source of heat (steam, electrical)

2. Dryers Description & Operation

Biopharmaceutical dryers: 1. 2. 3. 4. Vacuum-shelf dryer; Solids drying Vacuum-rotary dryer; Freeze dryer; Liquids drying Spray dryer.

We will find out: How they can be described? What are their working principles?

1. Vacuum-Shelf Dryer:
Operating principle:
- Trays filled with the product to be dried rest on shelves through which heating fluid is circulated. - Heat is conducted from the shelves to the trays and into the wet solids. - Vacuum is applied to the chamber containing the trays to speed up the drying and allow drying to take place at lower temperatures. - The evaporating water vapor is drawn off in the vacuum system.

Advantages: -Simple design;

-Cheap; -Reliable.

Disadvantage: -Case hardening.

2. Vacuum-Rotary Dryer:
Operating principle:
- Heat is supplied by heating medium circulated through a jacket on the rotating double-cone drum. - The solids are continually tumbled by rotation of the drum, so that solid particles come in contact with the walls of the jacket and with each other. - Vacuum is applied to the rotating drum to be able to dry at lower temperatures and to dry more rapidly.

3. Spray Dryer:
Operating principle:
- 4 stages involve in spray drying: 1. Atomization of feed into a spray of small droplets by atomizer provide large surface area for heat & mass transfer; 2. Contact btw droplets & hot air in the drying chamber; 3. Drying of droplets until desired dried particles are obtained; 4. Dried product recovery. - The character of the particles is controlled by droplet size, and so the type of atomizer is important.

Rotary atomizer

4. Freeze Dryer:

The product to be dried is normally in vials; A heat transfer fluid is circulated through the trays to provide temperature control of the vials. When the vials are first placed on the trays, the stoppers are closed only partially to allow water vapor to escape. The hydraulic piston allows the stoppers to be completely pushed into the top of the vials at the end of drying.

4. Freeze Dryer (contd)

Operating principle:
1. The product is first cooled to a sufficiently low temperature to allow complete solidification. 2. The pressure in the chamber is then reduced to below the vapor pressure at the triple point of water so that drying can occur by sublimation. 3. The temperature of the shelves is increased to provide energy for sublimation. 4. Condensation of vapor. 5. Dried product recovery.

Phase diagram for water

Applied to biological products, antibiotics, blood products, vaccines.

- Main advantage is operating at low temperature. - But slow (>24 hrs) & expensive.

Process variables during freeze drying