DRYING

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├── Definition
│ - Removal of small amount of liquid from a material by applying heat
│ - Heat is transferred from a surface into an unsaturated vapor phase
│ - Distinguished from evaporation by relative quantities of liquid removed
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└── Non-Thermal Methods
├── Expression of a Solid
│ - Squeezing of a wetted sponge
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├── Extraction of Liquid
│ - Use of a solvent to extract liquid from a solid
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├── Adsorption of Water
│ - Use of desiccants (e.g., anhydrous calcium chloride)
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├── Absorption of Moisture from Gases
│ - Passage through a sulfuric acid column
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└── Desiccation of Moisture
- Placing solid in sealed container with moisture-removing material (e.g., silica gel)

Purpose of Drying
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├── Preparation of Granules
│ - Tablets and capsules
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├── Specific Applications
│ - Dried aluminum hydroxide
│ - Spray drying of lactose
│ - Powdered extracts
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├── Bulk and Weight Reduction
│ - Lowering transportation and storage costs
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├── Preservation
│ - Minimizing mold and bacterial growth in animal and vegetable drugs
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├── Facilitating Comminution
│ - Making materials more friable
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└── Stability Improvement
- Effervescent salts, aspirin, hygroscopic powders, ascorbic acid, penicillin
- Reducing chemical reactivity
Purpose of Drying
│
├── Preparation of Granules
│ - Tablets and capsules
│
├── Specific Applications
│ - Dried aluminum hydroxide
│ - Spray drying of lactose
│ - Powdered extracts
│
├── Bulk and Weight Reduction
│ - Lowering transportation and storage costs
│
├── Preservation
│ - Minimizing mold and bacterial growth in animal and vegetable drugs
│
├── Facilitating Comminution
│ - Making materials more friable
│
└── Stability Improvement
- Effervescent salts, aspirin, hygroscopic powders, ascorbic acid, penicillin
- Reducing chemical reactivity

Psychrometry
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├── Determines
│ - Vapor concentration
│ - Carrying capacity of the gas
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├── Factors Affecting Drying
│ - Vapor-carrying capacity of the air
│ - Determines rate and extent of drying
│ - Lowest moisture content achievable
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└── Humidity
- Concentration of water vapor in a gas
- Referred to as the humidity of the gas
Psychrometry Chart Terms
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├── Psychrometric Chart
│ - Represents relationship between temperature and humidity
│ - Constant pressure system
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├── Axes Representation
│ - Horizontal axis: Temperature
│ - Vertical axis: Absolute humidity
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├── CDE Curve
│ - Saturation humidity
│ - RH = 100% (air fully saturated)
│ - Boundary of phase diagram
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├── FCA Dotted Line
│ - Absolute humidity (78 grains water/pound dry air)
│ - Represents relationship between temperature and pressure
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└── Dew Point (Point C)
- Temperature air becomes saturated with water vapor
- Cooling air to maximum moisture without condensation

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├── Point F (50°F)
│ - Mixture cooled below dew point
│ - Water vapor condenses into two-phase system
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├── Point A (81°F)
│ - Air not completely saturated
│ - Used for drying purposes
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├── Relative Saturation
│ - Ratio of absolute humidity (FCA) to saturation humidity (CDE) at same temperature
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├── GK Curve (50% RH)
│ - Curve at constant 50% relative humidity
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└── Wet-Bulb Temperature
- Equilibrium of heat transfer between air-liquid
- Measured by thermometer with bulb covered by saturated wick
Theory of Drying
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├── Heat and Mass Transfer
│ - Heat: Transferred into material for vaporization
│ - Mass Transfer: Diffusion of water to evaporating surface, then to air stream
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├── Rate of Evaporation Equation
│ - dW/dϴ = q/ƛ
│ - dW/dϴ: Rate of evaporation
│ - q: Overall rate of heat transfer
│ - ƛ: Latent heat of vaporization
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├── Driving Force for Heat Transfer
│ - Temperature differential
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├── Rate of Diffusion Equation
│ - dW/dϴ = kA(Hs - Hg)
│ - k: Coefficient of mass transfer
│ - A: Area of evaporating surface
│ - Hs, Hg: Humidity differential
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└── Coefficient of Mass Transfer
- Varied with air velocity over surface

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├── Rate of Drying Equilibrium
│ - After initial adjustment, heat transfer equals mass transfer rate
│ - dW/dϴ = q/ƛ = kA(Hs - Hg)
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├── Accelerating Drying Rate
│ 1. Increase Convection Heat Transfer
│ 2. Increase Radiation Heat Transfer
│ 3. Increase Conduction by Reducing Material Thickness
│ 4. Increase Air Velocity for Mass Transfer
│ 5. Dehumidify Inlet Air to Increase Humidity Differential
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└── General Principle for Efficient Drying
- Increase convection, radiation, and conduction rates
- Increase air velocity and reduce boundary layer thickness
- Dehumidify inlet air to increase humidity differential
Drying of Solids
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├── Moisture Representation
│ - Wet Weight: Water content as % of wet solid weight
│ - Dry Weight: Water content as % of dry solid weight
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├── Loss on Drying (LOD)
│ - %LOD = [(wt of water in sample / wt of wet sample)] × 100
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├── Moisture Balance
│ - Uses heat source to dry weighted wet sample
│ - Obtains %LOD
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└── Moisture Content (%MC)
- %MC = [(wt of water in sample / wt of dry sample)] × 100

Behavior of Solids during Drying/Rate of Drying

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├── Study of Drying Rate
│ - Crucial for understanding solid behavior during drying
│ - Determined by measuring weight of dry sample over time
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├── Drying Rate Analysis
│ 1. Drying rate vs moisture content
│ 2. Moisture content vs drying time
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└── Drying Rate Phases
├── Initial Adjustment Period (AB)
│ - Heating rate = Cooling rate until drying temperature stabilizes
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├── Constant Rate Period (BC)
│ - Moisture evaporates from surface, replaced by interior water diffusion
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├── Critical Moisture Content (C)
│ - No more moisture replacement, dry spot appears
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├── First Falling Rate Period (C-D)
│ - Drying rate steadily decreases
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├── Second Critical Point (D)
│ - Complete evaporation of surface film
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├── Second Falling Rate Period (D-E)
│ - Drying rate falls rapidly
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└── Equilibrium Moisture Period (E)
- Drying rate = Zero, temperature and moisture content remain constant
- Further drying is wasteful

Classification of Solids Based on Drying Behavior

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├── Crystalline Solids
│ - Water held in open surface pores and interstitial spaces
│ - Easily accessible to the surface
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└── Amorphous Solids
- Moisture integral part of molecular structure
- Entrapped in fine capillaries and pores
- More difficult to dry than crystalline solids
Types of Dryers
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├── Method of Heat Transfer
│ ├── Convection Dryers
│ ├── Conduction Dryers
│ ├── Radiation Dryers
││
├── Method of Sample Handling
│ ├── Static-bed Dryers
│ ├── Moving-bed Dryers
│ ├── Fluidized-bed Dryers
│ ├── Pneumatic Dryers
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├── Considerations
│ 1. Heat sensitivity of material
│ 2. Physical nature of material
│ 3. Nature of liquid to be removed
│ 4. Scale of operation
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└── Additional Notes
- Dryer design and energy requirement are important in the first classification
- Attention is given to the type of substance to be dried in the second classification

Static Bed System (Tray Dryer)

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├── Components
│ ├── Cabinet
│ ├── Shelves/Compartments
│ ├── Trays
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├── Operation
│ ├── Material spread on trays
│ ├── No particle movement
│ ├── Bulk motion only
│ ├── Exposed surface can be increased by decreasing bed thickness
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└── Advantages
- Simple operation
- Suitable for heat-sensitive materials
- Uniform drying across trays

Moving-Bed Systems (Turbo-Tray Dryers)

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├── Description
│ - Continuous shelf, moving-bed dryer
│ - Series of rotating annular trays in a vertical stack
│ - Trays rotate slowly at 0.1 to 1.0 rpm
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├── Heating and Air Circulation
│ - Heated air circulated by turbo-type fans
│ - Fans mounted in the stack center
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├── Operation
│ - Wet mass fed from the roof
│ - Leveled by a stationary wiper
│ - Dried material pushed through radial slots
│ - Transfers to the next shelf after each cycle
│ - Discharge at the bottom
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└── Advantages
- Faster drying rate than tunnel-dryers
- Continuous exposure to air enhances drying efficiency
Fluidized-Bed Systems
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├── Description
│ - Solids partially suspended in gas stream
│ - Mixture behaves like a liquid
│ - Solid is fluidized
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├── Application
│ - Used for drying granular solids
│ - Each particle surrounded by drying gas
│ - Intense mixing for uniform conditions
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└── Advantages
- High drying rate due to efficient heat and mass transfer
- Drying occurs at a constant rate with uniform heating
- Resultant granules are not wet or completely dried to prevent cracking
- Produces more spherical, free-flowing particles, reducing aggregation and color migration problems

Pneumatic Systems
Spray Dryers
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├── Description
│ - Handles fluid materials: solutions, slurries, and thin pastes
│ - Feeds fine droplets into hot gas stream
│ - Dried powder carried by gas current to collection system
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├── Process
│ - Liquid droplets contact hot gas, evaporating surface liquid
│ - Tough shell of solids forms quickly
│ - Shell becomes thinner, allowing faster diffusion
│ - Rupture produces intact spheres, spheres with buds, or fragments
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└── Characteristics
- Spray-dried material consists of various forms: intact spheres, spheres with buds, ruptured hollow spheres, or fragments

Spray Drying and Congealing

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├── Uses
│ - Drying heat-sensitive materials
│ - Changing physical form of materials (tablet and capsule manufacture)
│ - Encapsulating solid and liquid particles
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├── Applications
│ - Tablet and capsule formulations
│ - Coating and encapsulation of solids and liquids
│ - Sustained-release formulations
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└── Process
- Rapid drying with unique product form
- Drying process changes shape, size, and bulk density of the product
- Spherical particles flow better due to size and shape uniformity
- Chilling spray (congealing) used for taste masking and sustained-release formulations

Flash Dryers
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├── Description
│ - Moistened solid suspended in finely divided state
│ - Short-time drying process
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└── Operating Conditions
- Velocity: 3000-6000 feet/min
- Air stream temperature: 300-1300°F
Freeze Dryers
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├── Description
│ - Also known as lyophilization or sublimation
│ - Heat-sensitive materials dehydrated to solid state
│ - Frozen material subjected to high vacuum to sublime frozen liquid
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├── Examples
│ - Blood serum, plasma, antibiotics, hormones, bacterial cultures, vaccines, foodstuffs
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├── Reconstitution
│ - Dried product reconstituted by addition of water before use
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└── Sublimation Process
- Water passes directly from solid (ice) to vapor state
- Occurs below the triple point (4.579 mmHg and 0.0099°C)

Stages of Freeze Drying

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├── 1. Pre-freezing
│ - Material frozen below or at −20°C to avoid foaming
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├── 2. Vacuum
│ - Rotary pumps (small scale) or ejector pumps (large scale) used to reduce pressure
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├── 3. Primary Drying
│ - Latent heat of sublimation provided
│ - Vapor removed, primarily removing unbound water
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└── 4. Secondary Drying
- Removes bound water or traces of water left after primary drying
- Temperature raised (up to 50°C) or desiccant used for secondary drying

Microwave Drying
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├── Description
│ - Radical departure from conventional drying
│ - Energy in the form of microwaves converted into internal heat by material
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├── Heat Transfer
│ - Rapid heat transfer throughout material
│ - Moisture mobilized as vapor, not liquid
│ - Rapid movement to surface without mass concentration gradients or slow diffusion
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└── Advantages
- Extremely rapid drying
- Efficient heat transfer
- Reduced drying time compared to conventional methods