Lecture 6 Drying Unit Operations II Department of chemistry Collage of natural science In this Lecture… Basic principles and terminology in drying; Phase equilibria of drying process; Drying curve and drying rate curve under constant drying conditions; Material and heat balances, calculation of drying rates and drying time; Principles and structures of typical drying equipment. Introduction Drying is a complex operation involving transient transfer of heat and mass along with several rate processes, such as physical or chemical transformations, which, in turn, may cause changes in product quality as well as the mechanisms of heat and mass transfer. Physical changes that may occur include: shrinkage, puffing, crystallization, glass transitions. In some cases, desirable or undesirable chemical or biochemical reactions may occur leading to changes in color, texture, odor or other properties of the solid product. Drying occurs by effecting vaporization of the liquid by supplying heat to the wet feedstock. Over 85 percent of industrial dryers are of the convective type with hot air or direct combustion gases as the drying medium and Over 99 percent of the applications involve removal of water Drying, Introduction the mass and heat transfer operation that converts a solid, semisolid or liquid feedstock into a solid product by evaporation of the liquid into a vapor phase via application of heat. This definition excludes conversion of a liquid phase into a concentrated liquid phase (evaporation), mechanical dewatering operations such as filtration, centrifugation, sedimentation, supercritical extraction of water from gels to produce extremely high porosity aerogels (extraction) or so-called drying of liquids and gases by use of molecular sieves (adsorption). Phase change and production of a solid phase as end product are essential features of the drying process. An essential operation in the chemical, agricultural, biotechnology, food, polymer, ceramics, pharmaceutical, pulp and paper, mineral processing, and wood processing industries. Cont… Needed for the purposes of preservation and storage, reduction in cost of transportation, etc. Over four hundred types of dryers have been reported in the literature while over one hundred distinct types are commonly available. It competes with distillation as the most energyintensive unit operation due to the high latent heat of vaporization and the inherent inefficiency of using hot air as the (most common) drying medium. National energy consumption for industrial drying operations – 10-15% USA, Canada, France, and UK – 20-25% Denmark and Germany – ??? Ethiopia (Energy audit data not available) Why drying? Need for easy-to-handle free-flowing solids Less than 10% moisture microorganisms not active Usually dry to less than 5 % to maintain asls Preservation ,storage and elimination product deformation with time, Reduction in cost of transportation, Achieving desired quality of product, etc Drying makes materials more convenient in packaging, transporting, preserving, fabricating, and applying; and improves quality of products. Drying application Agriculture, dry Fruit and vegetable, Chemical industry, Detergent powder Pharmaceutical powder Ceramic and polymer Features of drying Product size may range from microns to tens of centimeters (in thickness or depth) Product porosity may range from zero to 99.9 percent Drying times range from 0.25 sec (drying of tissue paper) to five months (for certain hardwood species) Production capacities may range from 0.10 kg/h to 100 t/h Product speeds range from zero (stationary) to 2000 m/s (tissue paper) Drying temperatures range from below the triple point to above the critical point of the liquid Operating pressure may range from fraction of a milli-bar to 25 atmospheres Heat may be transferred continuously or intermittently by convection, conduction, radiation or electromagnetic fields Classification of Drying 10 Drayer types classification Criteria Mode of operation Batch Continuous* Heat input-type Convection*, Conduction, radiation, Electromagnetic fields, Combination of heat transfer modes Intermittent or continuous* Adiabatic or non-adiabatic Cont’d State of material in dryer Stationary Moving, agitated, dispersed Operating pressure – Vacuum* – Atmospheric Drying medium (convection) – Air* – Superheated steam – Flue gases Drying temperature Below boiling temperature* Above boiling temperature Below freezing point Relative motion between drying medium and drying solids Co-current Counter-current Mixed flow Number of stages Single* Multi-stage Residence time Short (< 1 minute) Medium (1 – 60 minutes) Long (> 60 minutes) Why so many dryer types? Over 500 reported in literature studies; over 100 commercially available Over 50,000 materials are dried commercially at rates of a few kg/hr to 30 T/hr or more Drying times (residence times within drying chamber) can range from 1/3 sec. to months Temperature and pressure range from below triple point to super-critical Numerous constraints on physical/chemical properties of feed as well as dried product require a bewildering array of dryer designs Wide range of feeds (liquid, solid, semi-solid, particulate, pasty; sludge-like; sticky etc); wide specs on dried product Cont’d Different sources of energy input( conduction, convection, radiation, MW,RF etc) Energy input continuous or intermittent Batch, continuous or semi-continuous operation Quality is key parameter for many products Limited number used in pharma industry Need to reduce the cost Need to consider drying system rather than dryer, i.e. Pre- and post- drying stages are important and often cost more than dryer Environmental regulations demand new drying techniques Criterion for selection of dryers Numerous criteria , with different weights Many dryers can typically meet specs; hence several dryers can do a given job in general. Mode of operation, Physical form of feed and dried product desired; heat sensitivity; quality requirements; production rate; whether non-aqueous solvents are present in feed; whether material is toxic/inflammable or friable etc Energy, environment, safety and cost. Products -quality is NO 1 criterion! As a minimum, the following quantitative information is necessary to arrive at a suitable dryer: Dryer throughput; mode of feedstock production (batch/continuous) Physical, chemical and biochemical properties of the wet feed as well as desired product specifications; expected variability in feed characteristics Upstream and downstream processing operations Moisture content of the feed and product Drying kinetics; moist solid sorption isotherms Quality parameters (physical, chemical, biochemical) Safety aspects, e.g., fire hazard and explosion hazards, toxicity Value of the product Cont… Need for automatic control Toxicological properties of the product Turndown ratio, flexibility in capacity requirements Type and cost of fuel, cost of electricity Environmental regulations Space in plant • For high value products like pharmaceuticals, certain foods and advanced materials, quality considerations override other considerations. • In some cases, the feed may be conditioned (e.g., size reduction, flaking, pelletizing, extrusion, backmixing with dry product) prior to drying which affects the choice of dryers • As a rule, in the interest of energy savings and reduction of dryer size, it is desirable to reduce the feed liquid content by less expensive operations such as filtration, centrifugation and evaporation. It is also desirable to avoid over-drying, which increases the energy consumption as well as drying time. Drying of food and biotechnological products require adherence to GMP (Good Manufacturing Practice) and hygienic equipment design and operation. Such materials are subject to thermal as well as microbiological degradation during drying as well as in storage If the feed rate is low (< 100 kg/h), a batchtype dryer may be suited. Note that there is a limited choice of dryers that can operate in the batch mode Typical check list for selection industrial dryers Cont. Conventional Vs innovative techniques selection Why select dryer carefully? Can affect bottom-line.. Product quality , energy usage affected by choice Expert systems exist for selection. Different expert systems give different selections Know product and process well before choosing drying system; imitation can cause problems! Simple decision trees suggested (SPS) Difference between drying and evaporation 1- In drying processes, the main operation usually carried out on solid materials, e.g. powders, or products. 2- Drying in most of the cases means the removal of relatively small amounts of water from solids .Evaporation include the removal of large amounts of water from solutions. 3- In most cases, drying involves the removal of water at temperatures below its boiling point, whereas evaporation means the removal of water by boiling a solution. 4- In drying , water is usually removed by circulating air over the material in order to carry away the water vapour , while in evaporation , water is removed from the material as pure water vapour mixed with other gases. 25 Drying equipments Types of Dryers Dryers for dilute solutions, suspensions and slurries a) Drum dryer b) Spray dryer Dryers for damp solid materials a) Tray or shelf dryer b) Tunnel dryer c) Rotary dryer d) Fluidized bed dryers (FBD) e) Vacuum dryer f) Freeze dryer PH 101.58 27 Tray dryer • • • • • • Rectangular chamber containing two truck that support racks (H) that load material to dry Rack contain shallow trays: 750mm square and 50-150mm deep Air velocity: 2-5 m/s by fan (C) and motor (D) Baffles (G) distributes air uniformly over the stack of trays Make up air added through exhaust duct (B) Disadv: – – – – • Used when production rate is small High labor cost for loading and unloading Expensive to operate Drying by circualation of air is slow and drying cycles – 4-48 h per batch Applications: drying of valuable products- dyes and pharmaceuticals Screen conveyer dryer • • • • Layer 25-150 mm thick dried slowly carried on a traveling metal screen through a long drying chamber Chamber contain series of separate sections each with its own fan and heater At inlet air is passed upward through screen and at discharge to prevent loss of dusty dried material air is passed downward Typical specifications: – • Adv: – – – • 2 m long and 4-50m wide, drying time 5120min, minimum screen size = 30 mesh Handle variety of solid continuously Reasonable cost Steam consumption low Application: – When the drying conditions must be appreciably changed as the moisture content of solid is reduced. Screw Conveyor Dryers • Continuous indirect heat dryer • Horizontal screw conveyor enclosed in a cylindrical jacketed shell • Solid fed in one end is conveyed slowly through the heated zone and discharges from the other end • Specification: – Shell 75-600 mm dia, 6 m long, rate of rotation = 2-30 r/min, heat transfer coefficient = 1560W/m2 oC • Applications: – For solids that are too fine and too sticky for rotary dryer Screw Conveyor Dryers Tower dryers • Series of circular trays mounted one above the another on central rotating shaft • Solid feed dropped on the topmost tray is exposed to stream of hot air that passes across the tray • Solid is scraped off and dropped to tray below • Specifications: – Air velocity: 0.6-2.4 m/s • Bottom two trays act as cooling section for dry solids • functions partially by cross circulation drying as in tray dryer and partly by showering the particles through the hot gas as they tumble from one tray to another Rotary Dryer • • • • Revolving cylindrical shell, horizontal or slightly inclined Wet feed enters one end of cylinder, dry material discharges from other As the shell rotates, internal flights lift the solid and shower them down. While in contact with the shell it gets heated by external jacket, during showering, it gets heated by direct contact with gas Typical specification – Allowable mass velocity = 2000-25000 kg/m2h – Inlet gas temp = 120-175 oC for steam heated air and 550-800 oC for flue gas – Diameter = 1-3 m – Peripheral speed of the shall = 20-25 m/min Rotary Dryers have many applications but are most commonly seen in the mineral industry for drying sands, limestone, stones and soil, ores, fertilizers, wood chips, coal, iron sulphate, filter cakes, sewage sludge, etc Rotary Dryer . Fluid bed dryer • Solid fluidized by drying gas • Wet feed is admitted to the top of the bed; dry product is taken out from the side, near the bottom • Velocity should be greater than the settling velocity of the particles • Particles are lifted in the gas stream • Average particle stay: 30-120 s when only surface is to be evaporated; 15-30 min if internal diffusion • Care must be taken for small particles as problem of carry away is severe. Advantage of FBD High rates of moisture removal due to excellent gas-particle contact which results in high heat and mass transfer rates. High thermal efficiency is usually achieved if part of the thermal energy for drying is supplied by the internal heat exchanger Lower capital and maintenance cost Reduced contact time for drying. Ease of control The conventional hot air fluidized bed dryer is not a good choice of dryer when handling toxic or flammable solids since there is danger of fire or explosion of flammability limits are exceeded. Disadvantage FBD High pressure drops results as a result of the need to suspend the entire bed in gas which equally leads to high energy consumption. Requires increased gas handling due to extensive recirculation of exhausts gas for high thermal efficiency operation. Poor fluidization and low flexibility especially if the feed is too wet. Not the best choice of equipment when organic solvents need to be removed during drying. Non uniform product quality for certain types of fluidized bed dryer. Entertainment of fine particles. FBD Flash dryer • Wet pulverized solid is transported for few seconds in hot gas stream • Rapid drying with drying time 3-4 sec • Temperature of gas too high 650 oC at inlet • Too small contact time rarely raised temperature of solid above 50 oC • Application To sensitive materials that in other dryers would have to be dried indirectly by a much cooler heating medium Spray dryer: for solution and slurries Slurry or liquid solution dispersed into a stream of hot gas in the form of mist of fine droplets • Moisture rapidly vaporized from droplets leaving residual particles of dry solid • Droplets formed by pressure nozzles • To prevent droplets or wet particles of solid from striking solid surface, diameter is made large (2.5-9 m) • Specification: • Spray disk = 300mm, rotates at 500010000 r/min • Gas leaving is passed to cyclone for removal of entrained solid • Cylindrical chamber is having conical bottom to collect the solids Drum dryers • • • • • • • Heated metal rolls on the outside of which a thin layer of liquid is evaporated to dryness Dried solid is scraped off the rolls at they slowly revolve Application Effective with dilute solutions, concentrated solution of highly soluble material and moderately heavy slurries Disadvantage – Not suitable for solutions of salts with limited solubility or for slurries of abrasive solids that settles out and create excessive pressure between drums Specifications 0.6—3 m dia, 0.6-4m long, revolving at 1-10 r/min, time for solid contact = 6-15 s, HT coeff= 1200-2000 W/m2oC, drying capacity = 5-50 kg per square meter of dryign surface per hour Freeze Drying It is known as sublimation drying It is also known as lyophillization as the dried product has great affinity for water ( lyophillic = water loving) is a low temperature dehydration process which involves freezing the product, lowering pressure, then removing the ice by sublimation. Freeze drying results in a high quality product because of the low temperature used in processing.The original shape of the product is maintained and quality of the rehydrated product is excellent. PH 101.60 42 Cont.. Freeze-drying does not usually cause shrinkage or toughening of the material being dried. In addition, flavours, smells, and nutritional content generally remain unchanged, making the process popular for preserving food. However, water is not the only chemical capable of sublimation, and the loss of other volatile compounds such as acetic acid (vinegar) and alcohols can yield undesirable results. Components of Freeze dryer Chamber for chilling the sample A vacuum source A heat source A vapor removal system Fig: 60.1 PH 101.60 44 Application of freeze drying Pharmaceuticals and biotechnology Freeze drying of food Process It is carried out for batch process The product is frozen first by putting on a shelf circulating refrigerants After freezing, vacuum is applied to the chamber Mild heat is supplied to the product by electric coils or by circulating hot water Process is continued till a dry, spongy solid is obtained PH 101.60 46 Products to be freeze dried are sterilized and aseptically distributed into final containers Container kept open during the process and sealed immediately after drying process PH 101.60 47 Advantages • The product is light, porous with good solubility • No chances of hydrolysis because, drying is at low temperature • No chances of oxidation because of no contact with air • Freeze dried products are more stable than vacuum dried product PH 101.60 48 Disadvantages • Very expensive • Time taking process • Dried product is very hygroscopic and requires special packing precautions PH 101.60 49 Uses • Mostly suitable for highly thermolabile products • Used for drying biological products such as blood plasma, vaccines enzymes, microbiological cultures, hormones and antibiotics and food ( ice cream, etc) PH 101.60 50 5.2 Terminologies pertaining to drying operations Moisture content of wet solids The moisture content of a wet solid is expressed as kilograms of moisture associated with 1 kg of the moisture – free solid. Thus a moisture content of 0.4 means that 0.4 kg of removable water is present per kg of the solid. It is sometimes calculated as percentage moisture content. Total moisture content: This is the total amount of liquid associated with a wet solid. The easily removable water is known as the free moisture content, and the moisture which is more difficult to remove is the equilibrium moisture content. The easily removable water is known as unbound water. Unbound water: This water exists as a liquid and exerts its fully vapour pressure, it can be removed readily by evaporation. During a drying process this water is easily lost but the resulting solid is not completely free from water molecules. 51 Equilibrium moisture content: • The moisture content present in a solid under steady-state ambient conditions is termed the eq. moisture content. Its value changes with temperature, humidity and the nature of the solid. Bound water : • Part of the moisture present in a wet solid may be adsorbed on surfaces of the solid or be adsorbed within its structure to such an extent to prevent it from developing its full vapour pressure and from being easily removed by evaporation. Such moisture is described as “bound” and is more difficult to remove than unbound water. 52 definitions 53 Definitions (cont..) 54 Definitions (cont..) 55 Definitions (cont..) 56 Relative humidity (RH) of air • Air at a given temperature is capable of taking up water vapour until it is saturated (at 100% RH ). If the temperature is raised then the air will be able to take up more moisture and the relative humidity falls. • The RH of air is dependent not only on the amount of moisture in the air , but also on its temperature, as the amount of water required to saturate air is itself dependent on temperature. • It should be noted that in convective drying, where warm air is passed over the surface of a wet solid, the relative humidity may rise during the drying process as a result of two separate factors:• 1- Uptake of evaporated water vapour from the wet solid, • 2- The cooling of the supply air as it transfers heat to the wet solid (evaporative cooling). • If the cooling is excessive the temperature of the air may fall to a value known as the dew point, when liquid water will condense and be deposited. 57