FLUIDIZED BED PROCESS FOR MAKING BEVERAGE, FOOD OR THE LIKE

Abstract: Absorption drying provides a means for agglomerating dried food and beverage solids around an aroma/flavor core, thereby essentially encapsulating said core and pre serving volatile flavor and aroma compounds. The absorp­ tion drying process is especially useful for manufacturing instant coffee. Thus, a viscous liquid extract comprising cof­ fee aromas and flavors is sprayed into a fluidized bed of instant coffee powder. Encapsulation of the coffee extract occurs as multiple particles of the coffee powder attach themselves to the aroma/flavor droplets to form aggregates. Rapidly drying the aggregates preserves the aroma/flavor in the core of the aggregates until released during use.

Description: s?LUIDZED BED PROCESS FOR MAKING BEVERAGE, FOOD OR THE LIKE This Invention encompasses a process for capturing and etaining aromas and/or flavors of the type found in foods anc beverages, and the compositions secured therefrom. The process herein is especially useful in the manufacture of beverages, particularly instant coffee. Commercial instant coffees are made by aqueous extracts of roast and ground coffee, followed by one of two basic drying processes. The older andgless expensive process involfl spray-drying the water extract. Unfortunately, volatile aroma and flavor components can be lost during spray-drying, and spray-dried instant coffees are generally characterized a less flavorful and aromatic than roast and ground coffees. Freeze-drying of coffee extracts is a more expensive process, but does generally yield a higher quality product with better aroma retention than spray-dried coffees. The present invention involves spraying small drops of aroma/flavor concentrates into a fluidized bed of dry coffee solids. Each atomized droplet is coated with dry -coffee solid to "lock in" the desirable aromas and flavors. This process is termed "absorption drying" herein. The absorption drying process of this invention provides a loer-cost alternative to freeze-drying. By operating in a concentrated system composed of an aroma-rich core surrounded by a dry shell, the retention of volatiles during absorption drying is the same or better than with freeze-drying. It is to be understood that the adsorption drying process of this invention is not limited to the manufacture of instant coffee but can be used in the manufacture of a wide variety of instal foods, beverages and the like. In particular, instant grain beverages having excellent coffee-like aromas and flavors can be made hy the present process, as can instant teas, instant fruit-flavored beverages, instant chocolate beverages, instal sups, and tulle like. Background Art Hair, Cody and McLain, U.S. Patent 3,615,669, issued 1971, disclose a fluidized bed agglomeration pro- cess for manufacturing coffee. U.S. Patent 3,903,295, issued 1975, discloses a process for encapsulating materials which tend to degrade within a film-forming agent. Thijssen, H.A.C., "The Effect of Process Variables on Aroma Retention in Drying Coffee Extract", ASIC, June 2-6, 1969; and Thijssen, H.A.C., "Effect of Process Conditions in Drying Coffee Extract and Other Liquid Foods cn Aroma Retention", ASIC, June 1973, relate to studies of the mass transport properties of model aroma compounds during a coffee drying operation. Chandrasekaren, S.K. and King, C.J. address the topic of "Volatiles Retention During Drying of Food Liquids", AIChE J., 18, pp. 520-526, 1972. Rulkens, W.H. has considered the "Retention of Volatile Trace Components in Drying Aqueous Carbohydrate Solutions" in his Ph.D. Thesis, Eindhoven University of Technology, 1973. Chandresekaren, S.K. and Ring, C.J. discuss diffusion of volatiles in their article "Multicomponent Diffusion and Vapor-Liquid Equilibria of Dilute Organic Components in Aqueous Sugar Solutions", AIChE J., 18, pp 513-520, 1972. Additional work in the area of the retention of volatiles is reported by Rulkens, W.H. and Thijssen, H.A.C., "The Retention of Organic Volatiles in Spray- drying Aqueous Carbohydrate Solutions", J. of Food Tech. 7, pp. 95-105, 1972. Kerkhof, P.J.A.M. and Schoeber, W.J.A.H., Advances in Preconcentration and Dehydration of Foods, As Spicer (ed.), Applied Science Publishers Ltd., London, 1973, p. 349 and Rulkens, W.H. and Thijssen, H.A.C., Trans. Inst. Chem. Engrs., 47, p. 292, 1969 are relevant to the 1; general topic of volatiles retention. Uemaki, O. and Mathur, K.B., "Granulation of Ammonium Sulfate Fertilizer In a Spouted Bed", Ind. Enq. Chem. Process Des. Dev., 15, pp. 504-508, 1976, disclose fluidized bed processes for fertilizer granulation. The abstraction and capture of volatile aroma and flavor materials frorn coffee and other edibles such as oranges are disclosed in U.S. Patents 3,595,669; 3,717,472 and 3,997,685, to R.G.K. Strobel. The Strobel procedures can be used to prepare the aroma and flavor concentrates used in the present process. U.S. Patent 3,704,132, to Strobel, discloses a method for purifying coffee oil for use as a coffee aroma carrier. Coffee extracts of the type used herein c?n be prepared by various art-disclosed means, including that described in U.S Patent 3,700,466, to Bergeran and Schlichter, and in U.S. Patent 3,700,463, to Bolt and Strobel U.S. Patent 3,625,704, to Andre, Joffe and Strang, discloses a means for preparing instant coffee in the form of flakes. U.S. Patent 3,769,032, to Lubsen, Strobel, Reinbart and Patel, discloses a means for preparing aroma-enriched coffee products. Several U.S. patents disclose means for preparing spray-dried coffee particulates and other instant foods and beverages. See U.S. Patents 2,771,343; 2,750,998; and 2,469,553. See also Sivetz and Foote, "Coffee Processing Technology", Avi Publishing Co., 1963. The foregoing U.S. patents and references disclose means or preparing various components used in the prac tice of the present invention, and are incorporated herein by reference. Disclosure of the invention The present invention provides a process for manufacturing a water-dispersible composition for use as an instant food instant beverage, or the like2 characterized by: à) atomizing a liquid aroma concentrate, A flavor con pentrate, cr a mixed aroma/flavor concentrate, commensurate with said food, beverage or the like, and having a viscosity of from 5 centipoise to about 200,000 centipoise, as droplets into a fluidized bed, the solids in said fluidized bed com- prising a multiplicity of particles, or mixtures of particles and flakes, comprising a dried extract of said food, beverage, or the like, at a ratio of droplets: :solids of at least 1;5 by weight, whereupon said particles and flakes form aggregates on said droplets, said aggregates having a moisture content less than about 15%; and (b) drying said aggregates substantially immediately after their formation to a moisture level of less than about 10%, preferably to a level in the range from about 2.5% to about 4.5%, especially from about 3.0° to about 3,5. Drying the aggregates quickly, i.e., substantially immedi- ately after their formation and recover, is critical fcv , securing products having optimal aromas and flavors. Moreover, overall product aroma and flavor are optimized by performing the process under conditions such that a dried shell forms quickly around the aroma/f lavor-rich droplet. Aroma an- flavor components are impermeable to the dried shell and thus are retained in the product aggregate throughout the process. These observations are in accord with the reports by Thijssen (above), and reflect the fact that the diffusivity of aroma and flavor in a coffee extract system is dependent on the water concentration. Thus, at lower water concentrations (ca. < 10% preferably < 3.5%), such as are present in the shell of the dried aggregate, the diffusivity of aroma-type compounds is three orders of magnitude less than the diffusivity of water. Indeed, the relative diffusivity of the aroma volatiles is so small that the shell can be considered as being selectively permeable only to water. Accordingly, by drying the aggregate products of the present processes as soon as possible after their formation, water is removed before the desirable volatiles can escape. The present invention alse enco-tDasses water-dispersible compositions for use as instant foods, instant beverages, or the like, said compositions being in the form of aggregates1 said aggregates comprising: (a) a core comprising an aroma concentrate, a flavor concentrate, or, preferably, a mixed aroma/flavor concentrate coir±nensurate with said foods, bever- ages, or the like, said core being substantially surrounded and encapsulated by; ; (b) a multiplicity of particles, flakes, or, prefer- ably, mixtures of particles and flakes conlprising a dried extract of said foods, beverages, or the like, merged on the outer surface of said core The -process of this invention is especially useful in the manufacture of instant coffee compositions in the form of aggregates, said aggregates comprising: (a) a core of coffee aroma or flavor materials, or, preferably, mixtures thereof, said core being substantially surrounded by and encapsulated hy; (b) a multiplicity of particles, flakes, or, prefer ably, mixtures of particles and flakes, of dried coffee extract, merged on the outer surface of said core. Highly preferred coffee, etc., compositions herein are those wherein said aggregates contain no more than about 4.5% by weight of moisture and are.free-flowing. Highly preferred instant coffee compositions herein comprise the coffee aroma/flavor core surrounded and en capsulated by a mixture of dried coffee flakes and coffee particles merged to form an aroma/flavor encapsulating shell. The weight ratio of particles:flakes is in the range of from about 30:70 to about 70:30, generally about 60:40. Such coffee compositions most preferably contain no more than about 4.5% by weight of water, and are free flowing. All percentages herein are by weight, unless otherwise specified. Best Mod The following describes a preferred and convenient mode of practicing the present invention to manufacture an instant coffee product characterized by improved flavor and aroma qualities. It will be appreciated that the same method can be used to manufacture other instant beverages such as instant tea, instant fruit drinks, and the like At the heart of the process is a fluidized bed of spray-dried coffee particles. Alternatively, this fluidized bed can be a mixture of different types of dried solids, for example grain and coffee, to prepare a grain coffee beverage. The fluidized bed can have the solids in different forms; the solids are preferably a spray-dried instant coffee powder admixed with instant coffeefIakes The presence o' the flakes in the final aggregate product greatly improves product appearance and desirably enhances the strueL-ural integrity of the aggregates. Fluidization is a process wherein fine solids are made to behave in a fluid-like manner. Fluidization is accomplished by allowing a stream of gas (e.g., air, nitrogen, etc.) to rise through a bed of coffee parti elves. Fluidization will take place when the force of the fluidizing gas exceeds the force of the weight and friction factors within the bed of solid particles A dense phase fluidized bed behaves much like a boiling liquid, so a stream of atomized droplets of concentrated aroma/flavor can be introduced into the fluidized bed of Coffee1 whereupon the droplets are quickly coated. A convenient fluidized bed apparatus used to prepare pilot plant batches of adsorption dried instant coffee in the manner of this invention comprises a 15 cm I.b. vertical column ca. 1.435 m. in height with a Plexiglass viewing section at the lower bed portion and a stainless steel disengaging section. The gas (N2 or air) distributor for fluidizing the solids is a porous sintered metal disc comprising the base of the coluirin. The cas supply is a 1.2 cm. compressed air or N2 line supplying 80-100 psi. A spray nozzle is positioned centrally in thesintered disc and is directed upwardly to atomize the aroma/flavor liquid directly into the fluidized bed comprising the coffee particles and flakes. The exit port of the nozzle protrudes ca. 10.2 cm into the cylinder, the entrance port is connected to a reservoir of the liquid aroma/flavor concentrate. For an apparatus of the foregoing size the nozzle is 508 microns ( )/1270 (I.D./O.D.), with the air cap having a 1778 I.D. (Spraying System pneumatic nozzle). A nozzle of these dimensions provides a full cone 18 spray In operation, the cylinder is charged to ca. 158 of its height with coffee particles or flakes (ca. 0.65 kg.). Air or N is introduced into the column via the L sintered metal base to fluidize the bed of coffee. The concentrated aroma/flavor solution is then atomized through the spray nozzle into the dense phase fluidized bed of coffee, whereupon the desired instant coffee aggregates are formed. The aggregates (ca. 10-15% by weight water) are removed from the cylinder and dried, preferably within 1-2 minutes after removal, and within about 5 minutes after their formation, -to a moisture level -of ca. 2.5%- 4.5%, most preferably ca. 3.0%-3.5%, thereby locking in the aroma/flavor in the form of a core for the individual aggregates. It will be appreciated that the concentrated aroma/ flavor solution used in the foregoing manner should be somewhat viscous and tacky so that the solid coffee particles and flakes adhere to the atomized droplets. The solute content should be as high as possible, consistent with achieving the desired viscosity. An aqueous aroma/ flavor solution with a viscosity below about 5 centipoise (cps) is not useful in the practice of this invention Since the water with dissolved aroma/flavor solutes simpl wicks into the solids and does not form the desired struc ture comprising the core encapsulated by the shell formed is the particles and flakes merge. The viscosity range is dependent on the dissolved solutes in the aroma/flavor solution, and these solutes generally comprise ca. frcm about 30% to about 70% of the solution, which corresponds to viscosities in the range of from about 19 ops to about 200,000 cps. Preferably, the solut content' is ca. SO Preferably the viscosity is in the range of 500-700 cps It is highly preferred that the process of this invention be carried out using a mixture of instant coffee particles and instant coffee flakes, for several reasons First, a better quality of fluidization in the fluidized bed is achieved, presumably due to the broader range of sizes of the solids being fluidized. The presence of shiny coffee flakes in the final agglomerated product also contributes substantially to product appearance. For example, coffee products made in accordance with this invention containing coffee flakes have a rich, brown appearance. Other products made by this process, e.g.r orange juice beverage aggregates containing orange flakes, have a desirable sheen. Moreover, the flakes contribute importantly to the stability of the aggregates. During the fluidizing process, the aggregates being formed are continually subjected to abrasion until such time as they are removed fromathe fluidized bed and dried. It is important that the aggregates not disintegrate, since the aroma/flavor volatiles in their cores would be lost The presence of flakes in the aggregates helps maintain their integrity during formation. Moreover, the presence. of the flakes in the aggregates helps maintain aggregate integrity during the subsequent drying step, which preferably com- prises drying the aggregates while they are being vibrated The coffee particles used in the practice of this invention comprise spray-dried instant coffees. As manu factured, spray-dried coffee has an average particle size in the 5-300 micron range and the particles are hollow For use herein, the pray-dried coffee particles are pre-. ferably milled (and thereby densified) to a particle size in the 5-50 micron range The instant coffee flakes used herein are somewhat larder than the coffee particles The optimal flakes pass through a 16 mesh Standard Sieve. Flake manufacture .s described in U.S. 3,625,704 (above). The aggregation step of this process is carried out by atomizing the tacky liquid aroma/flavor concentrate into the dense phase of the fluidized bed of solid inst & t coffee Droplet size of the concentrate is in the 50-500 micron range, that is, slightly larger than the solid bed material. In general, 5 parts by weight of bed solids to 1 part of spray provide excellent agglomerates. The rat of introduction of the concentrate into the dense phase of the fluidized bed affects the rate of agglomeration. In the extreme, if the concentrate is atomized too rapidly, the individual droplets of concentrate coalesce, this is to be avoided. A convenient rate of atomization- for preparing instant foods and beverages'in a pilot scale apparatus as disclosed above introduces about 24 grams of the liquid aroma/flavor concentrate into the bed per minute. Thus, in a typical pilot-scale bed comprising 650 g. of 1.1 coffee particles and flakes, 130 g. of aroma flavor concentrate is introduced over a period of about 5 minutes and 23 seconds. It is highly preferred that the aggregates as prepared in the bed contain no more than about 10% to about 12 total moisture. If the moisture content is allowed to become greater than about 15% (e.g., by using slightly damp coffee solids as the bed material, by using excess water in the aroma/flavor concentrate, or by operating at too high a humidity), the aggregates are too tacky and begin to set up in a solid mass before they an a recover ed from the fluidizing apparatus. As disclosed below after aggregation is complete, the moisture content is further reduced by a drying step. The aggregation step of the present process is con leniently carried out at temperatures of about 20 C-30 C. If the fluidized bed is allowed to become too warm, desirable aroma and flavor volatiles can be lost. If the fluidized bed is run at extremely cold temperatures to minimize the loss of volatiles, longer drying times in the subsequent step are required. After the aggregates are formed, they are dried Proper control of the drying step is very important. I± X after they are formed the aggregates are allowed to stand for a substantial period of tine (ca. 3-5 minutes, or, perhaps, somewhat longer, depending on the surrounding conditions of temperature and humidity) the desirable aromatic and flavor volatiles in the core of the aggregates will migrate to the surface and be less. Accordingly, it is important that the aggregates be dried substantially immediately after they are formed and recovered from the fluidized bed. Again, this can depend somewhat on the moisture content of the core, but for aggregates which comprise about 105-125 moisture, drying should begin within about 1-2 minutes after the aggregates are recovered from the fluidizing apparatus. Preferably, a continuous fluidized bed apparatus is equipped with a standard col- lecting device so that, as the aggregates are formed, they are continuously removed and delivered directly to the dryer. Drying can be carried out in any manner which reduces the moisture content of the aggregates to the desired range quickly. Preferably, the drying tie for an individual aggregate is about one minute. Forced air, warm forced air (preferred: 90-100 C air), radiant heat, vacuum drying, and the like, can be used, as long as dryness is quickly achieved so that the shell of merged particles around the core "lock in" the volatile arorna/- flavor components. Whatever means of drying is used, it is important to aroma/flavor retention no to allow the temperature of the aggregates, themselves, to exceed about 70-75 C. Preferably, the aggregates are vibrated con tenuously during the hot air drying step. In an optimal (ca. one minute; 90-100 C) forced air vibratory drying step, the aggregates reach temperatures of about 60 C. Commercial apparatus such as the Jeffry Vibratory Dryer are convenient for use in the drying step of the present process. Industrial Applicability The practice of the present invention Is turtber illustrated by the following exemples, which are not tended to be limiting of the type of ngestible composi- - > ons which can be manufactured by the present process Example I In accordance with the procedure disclosed in U.S. Patent 3,997,685, a coffee column having a width of ca 12.7 cm. and a length of 15 cm. is placed in communication with two in-line condensing traps. The first trap is held at -76 C by dry ice. The second trap is held at -195.8 C by liquid nitrogen. A vacuum pump is connected to the system to allow the use of vacuum pressures during operation. 900 grams of roasted coffee beans are frozen in liquid nitrogen and ground to a fine grind size, i.e., less than 20. mesh U.S. Standard Sieve. In order to purge the system of oxygen, 10 grams of solid carbon dioxide are placed on the beans and allowed to sublime and be carried through the system to displace oxygen. The roast ad ground coffee is placed in the column. Water at 90 -100 C is introduced to produce wet steam which is pulsed downward through the column zone. The cold wet steam is passed in a downward manner through the column in a pulsing fashion 'and introduced at approximately two-minute intervals in approximately equal amounts. A black band of materials is evident in the uppermost portions of the column. During the run this band continually moves downward through the column prior to breakthrough. Prior to breakthrough, a colorless frost is collected in the first trap and retained. The second trap, which is held at liquid nitrogen temperatures, provides a solidified aroma frost which comprises coffee aroma and carbon dioxide solidified into an aroma-CO2 matrix. The melted frost from the two traps prepared in the foregoing manner is admixed with spray-dried cGffC'e solids to prepare a ca. 50% aqueous concentrate of total dis solved coffee solids, viscosity ca. 604 centipoise. The amount of aroma/flavor fluid used can be adjusted accord- 'ing to the needs of the formulation. An aroma/flavor concentrate having a viscosity in, the 600-700 cps rare 5 preferred. The 'aroma/flavor concentrate prepared in the fore- going manner is atomized into a fluidized bed comprising ca. 60% (wt.) of spray-dried instant coffee powder and ca. 40% (wt.) instant coffee flakes, using the apparatus and technique described hereinabove. Approximately 100 g. of aroma/flavor concentrate per 500 g. of the mixture of powder and flakes is used. As the aroma/flavor concentrate is atomized into the fluidized bed, the powder and flakes aggregate o the droplets to form aggregates. Said aggregates comprise ca. 10% water. The aggregates are imm.ediately removed from the fluidized bed column and heat-dried (Jeffry continuous forced air dryer; ca. 95-100 C air; average moisture con tent of ca. 3.5% b weight). The instant coffee product prepared in the fore going manner has a density of ca. 0.3 g./ml. One tea spoonful (1.5 g.) of the product added to 150 mls. of hot water rapidly dissolves to yield a flavorful, aromatic coffee beverage whose organcleptic properties are fully equivalent to freeze-dried instant coffee. Example II Coffee beans (25% Robusta; 75 Arabica) are decaf feinated with methylene chloride in standard Fashion, roasted, ground, extracted and the extract spray-dried and crushed to ca. 25 microns. A portion of the decaffeinated instant coffee is converted to flakes by roll milling in the manner disclosed in U.S. 3,625,704. A X1 (t.) mixture O the decaffeinated coffee particles and flakes is placed in a fluidizing apparatus, as disclosed above. An aroma/flavor concentrate (604 cps) is prepared using decaffeinated coffee solids in the manner of Example I. The concentrate is atomized into the dense region of the fluidized bed and aggregates. form. The aggregates are removed from the apparatus and sub- stantially immediately dried (hot air) to a moisture content of 3.52. The product is'a flavorful, aromatic decaffeinated coffee. Example III Using the aroma/flavor extraction procedure of Example I, peeled oranges are frozen in liquid nitrogen and finely ground to a mesh size of 7. The ground oranges are placed in the extraction column; 25 grams of carbon dioxide are placed in the system and allowed to sublime to purge the system of oxygen. During extraction, the system is continually flushed in a downward manner with carbon dioxide. 400 ml. of liquid flavor concentrate is collected in the first trap subsequent to breakthrough. The band which continually moves downward through the column as pulsing of the wet steam occurs is a bright, very intense orange color. The liquid flavor concentrate has a pleasant orange aroma. The liquid nitrogen trap contains a very pleasant but not especially intense orange aroma-cO2 matrix. The aroma and flavor materials thus prepared are combined for further use. An orange juice concentrate is spray-dried to a particle size of ca. 100-300 microns and crushed to ca. 50 microns. The orange powder thus obtained is fluidizing apparatus. The orange flavor/aroma materials prepared above are admixed with concentrated orange juice (ca. 1,000 cps) t' provide an orange flavor/aroma concentrate. The flavor/ aroma concentrate is atomized into the flidized bed of dried orange juice powder in the proportions disclosed in Example I. Aggregates form. The orange aggregates are dried within about 3 minutes after their formation to a moisture content of ca. 3t. When added to water (ca. 8.0 g. per 100 g. of water) the aggregates dissolve to provide a pleasant reconsti tuted orange juice beverage. The process of rx2mple III is repeated with tomatoes, limes, grapefruit, lemons, 1:1 lemon/lime mixed tures and chocolate (cocoa), respectively, and excellent instant beverage. products are secured. The instant tomato product of Example III is used at a level of ca. 15 5. per 100 g. of hot water to provide a tomato soup. Example IV Coffee-flavored grain beverages with excellent coffee aroma and flavor are prepared as follows. A. Preparation of Grain Extract Particles. A dry, refined grain extract is obtained from 500 g. of roasted and ground malted barley. The barley is placed into a ca. 12.7 cm. glass column. The glass column is closed with a disc-shaped lid. The lid is equipped with four openings -- a center opening and three additional openings symmetrically arranged around the center opening. The center opening is used for placing a nozzle above the barley substrate bed. The distance between nozzle opening and substrate bed is i5 cm. Two of the remaining three openings are used for placing thermocouples into and above the substrate bed for temperature measurements during the run (two openings). The remaining opening is used for connecting a nitrogen line to the column. The column is evacuated to an absolute pressure of 1 mm. h condensing trap is placed between the vacuum pump and the column to condense volatile materials from the barley bed. The condenser is cooled with liquid nitrogen The volatiles are driven off by pulling spurts of boiling H20 through the nozzle. The spurts of hot water are partially transformed into steam (approximately 20% steam transformation at 1 mm. vacuum). The steam trans- formation also cases a temperature reduction of the steam/water mixture to 20 C. The water is soaked up by the substrate, thereby causing the desorption of additional volatiles which are carried by-the steam through the substrate bed (steam distillation). The volatiles and steam distillable volatiles condense in the trap. Addition of subsequent water/steam spurts (s 10 ecin. each) onto the substrate pushes the aqueous front deeper into the substrate bed, causing the desorption of added tional volatiles, etc. After ca. 13 minutes, a total of 900 ml. of water is introduced onto the substrate bed, at which point the aqueous front reaches the lower end of the. substrate bed. Now, the condenser containing the volatiles and steam-distillable materials is replaced by a fresh condenser. The volatiles are discarded. Addition of subsequent water (spurts) onto the substrate bed causes the aqueous front, which contains water-soluble refined grain extract (pigments, carbohydrates, proteins, inorganic components, etc.) to exit into the new condenser. The new condenser is placed into a dry ice/solvent mixture. After 30 minutes, 1.9 liters of hot H20 will have been introduced onto the substrate bed. 1029 ccm. of H2V- soluble grain solids are collected in the trap {draw-ofr ratio 1:2.06 ratio 1:2.06). The aqueous malted barley extract is spray-dried, rìlled., and sieved. The dry refined grain extract ex hibits a bland flavor. In an alternate mode, grain such as roasted rye, wheat or malted barley is extracted with water in a coffee extract colmn, concentrated and spray-dried to form soluble grain extract particles. The dried, soluble grain extract particles prepared in the foregoing manner are used to prepare a coffee flavored instant beverage composition by absorption drying in the manner of this invention by both of the following procedures. Procedure 1. An aqueous aroma/flavor coffee con pentrate prepared in the manner of Example I is atomized into a fluidized bed of the roasted grain particulates prepared as described hereinabove using the apparatus disclosed herein. The ratio of aroma/flavor concentrate to dry grain particles is adjusted so that about 200 rng. of the concentrate per gram of soluble grain particles is used in the absorption drying process. Processing in tha fluidized bed apparatus yields aggregates which comprise a tacky, coffee-flavored core surrounded by the soluble grain particulates. Within about 2 minutes of their fornraticn, the coffee-flavored grain beverage aggregates are removed from the fluidized bed apparatus and dried (forced hot air dryer, as disclosed above; average resi dence time per aggregate ca. 1 minute). The coffee-flavored grain beverage product prepared in the foregoing manner is added to hot water at a level of about 1.1 ó and provides a coffee-flavored beverage. Procedure 1 is repeated by replacing the coffee flavored extract with viscous aroma/flavor extracts (650 cps) of tea, beef, oranges, cola nuts, and lemons, re spectively. The resulting aggregates are suitable for use as instant beverages, soups and foods. Procedure 2. The coffee-flavored grain beverage product prepared by Procedure 3 provides a quite acceptable beverage, but does not provide all the aroma and flavor characteristics demanded by the most discriminating coffee drinkers. The following procedure provides a highly flavorful and aromatic coffee concentrate which is used to manufacture instant coffee products which are virtually indistinguishable from high quality, 100 coffee beverages Preparation of Coffee for Desorption of Aroma and Flavors. Tazenty-five kg. of coffee beans are roasted to a photovolt reading of 70 and quenched, first Widl one liter of water and then with liquid nitrogen. The water quenching is carried out in the roaster ("Probat" roaster) Immediately after water-quenching, the beans are placed in metal drums and shock-quenched with 20 kg. of liquid nitrogen t6 a temperature of Ç -100C. One kg of powdered dry ice is mixed into the quenched beans before grinding. The beans are then ground to a coarse grind (instant coffee grind) and then immediately milled on a "Ross" mill with a distance of 88.9 microns (3.5 mils) between rolls. Hydraulic pressure on the rolls is Ca. 350 lbs. Speed of the rolls is ca. 100 rpm. Rolled coffee flakes are secured. Desorbate Column and Ancillary Equipment. A Desorbate Column for capturing aroma and flavor components is assembled and consists of four components. 1. A cylindrical section 60 cm. in diameter and 50 cm. high. Both ends of this section are ground 2. A top section, dish-shaped with four openings, receiving a nozzle system for steam/water appli cation, C02-purging, and thennocouples for temperature measurements. A hot water reservoir is connected to the nozzle system. A solenoid valve is placed between the hot water reservoir and the nozzle system. The tcp section is placed on a stainless steel n'ing plate that provides, via two O-rings, a eJacuum-tight seal between the cylindrical and top sections. The stainless steel ring also providers a means for lifting the top section for filling and discharging the column. 3. A false bottom, consisting of a 55% perforated stainless steel plate placed between the cylin- drical section and the bottom section. Two 0 rings provide a vacuum-tight seal between the two sections. Seven layers of cheesecloth are placed on the perforated plate to prevent the flaked coffee from falling through when loading the column. 4. A dish-shaped bottom, equipped with a valve. The valve extends via vacuum tubing to a condensing system. The condensing system is connected to a mechanical vacuum pump. The pump is protected against water vapors with two cryogenic traps. The three column sections, made of "Duran" glass, are held together by metal flanges. The metal flanges are connected to a tubular frame system supporting the entire column setup. Loading and Purging the Column. The lid section is lifed with a mechanical winch and 20 kg. of rolled coffee flakes prepared as disclosed above are placed onto the false bottom (cheesecloth). The rolled coffee flakes are spread out to obtain- a level bed surface in parallel with the false bottom plate. The lid is then lowered onto the cylindrical section and the air above the coffee bed is displaced with CO2. Preparation of Aroma/Flavor-Frost Condensinq Vessels The condensing system consists of three 8-liter cylindrical flasks (18.7 cm. diameter) placed in parallel between the Desorbate Column and the vacuum source. The condensing vessels are placed into liquid nitrogen. Each condensing vessel is coated cn the inside with 300 grams of a 60% solution of "Desorbate' coffee base extract obtained froiit a previous run (180 grams Desorbate base dissolved in 120 ml. of distilled water). The concentrate is poured into the cylindrical vessels and the vessels are then rotated in a near horizontal position until an even coating of concentrate is achieved on the inside walls. The vessels are then quickly placed into the liquid nitrogen to freeze the even coating. Evacuation of Colw=n. After displacing the air from the column and connecting the condensers to the column on the one side and to the vacuum pump on the other side, the vacuum pump is turned on. The bottom valve of the column is slightly opened to prevent the highly volatile materials from rushing through the condensing system. Evacuation of the column under these delayed conditions takes about 10 minutes. Desorption and Condensing of Aroma/Flavor Frost. After evacuating the column to 1 Torr, the solenoid valve is opened by an electrical switch for approximately one second. One-haft liter of water from the reservoir is pulled into the nozzle system. The nozzle system produces en even spray pattern over the coffee bed. The vacuum in the column causes part ( 20%) of the hot water (990C) to transform into steam. The transformation into steam is accompanied by a temperature drop of the steam/water mixture from 99 C to 20 C. The water is immediately soaked up by the rolled coffee flakes and in turned desorbs volatile gases like and offee aroma/flavor compounds from the rolled coffee flakes. The evaporation of the volatiles can be visually observed by the formation of gas bubbles at the interface between the wetted part and the dry part of the bed of rolled coffee flakes. As soon as the formation of gas bubbles subsides, bother spurt of hot water is introduced onto the column his This spurt drives the interface deeper into the The bed The interface develops without any channeling uneven migration into the coffee bed. As soon as the rolled coffee flakes are saturated with water, dissolution of soluble materials into the aqueous phase occurs, as evidenced by the formation of a dark brown band of solubles. This dark brown band moves 'deeper into the coffee bed and renewed activity of volatiles desorption occurs when additional spurts of water are applied. The subsequent Table gives detailed information on various parameters like temperature in and above the coffee bed, the vacuum at the interface and above the column bed, the quantities of water applied, the tine elapsed, etc. Table I Various Desorbate Parameters Temperature C Hot Head Top Water Time Vacuum of Added (Min.) (Torr) Above Bed Bottom (liters) Remarks 000 1 2 -7 -7 00.0 ) C02-purging 007 40 30 30 15 08 ) 010 40 36 36 36 10 ) Collection of ) Aroma/Flavor ) Frost 015 80 46 46 46 14.5 ) 025 100 50 50 47 22.5 ) 030 100 46 50 46 23.0 ) Break Through 040 90 46 45 42 5.0 ) Collection of 055 90 52 50 49 33.0 ) 1st cut 075 100 50 48 47 39.0 ) Collection of 085 90 49 48 47 42.0 ) base material 090 95 49 49 47 46.0 ) 110. 90 The volatiles consist of C02, aroma/flavor compounds desorbed fro the rolled coffee flakes,and steam. The volatiles produce a vJhitish-slightly yellow layer of aromas flavor frost in the condensers. (The condensers are protected against light during collection of the aromas flavor frost.) As shown in Table I, the collection of the aroma/ flavor frost is finished after 30 minutes run-time and application of 23 liters of hot water through the nozzle system. At this time, the interphase begins to "break through" the layers of cheesecloth. At this point the aroma/flavor frost traps are removed from the column system. The traps are sealed with cellulose plugs and kept in the dark in liquid nitrogen jackets until use. Each of the three aroma/flavor frost traps contains about 400 ge of frost. Preparation of Coffee Aroma/Flavor Concentrate. Approximately 340 g. of soluble coffee solids are aded to each trap to yield a coffee aroma/fl2vor concentrate con tanning ca. 50% total coffee solute (including coffee solids used to coat the traps). 'The 2roma/flavor concentrate prepared in the fore- going manner is atomized into a fluidized bed of soluble grain particles. The aggregates which form are quickly dried to a moisture content of ca. 3.5t, and are freeflowing. A 1% aqueous solution cf the aggregates provides an excellent "coffee" beverage. The aroma/flavor concentrate of Example II is sub stantially caffeine-free and can be used in the foregoing manner to manufacture a decaffeinated instant grain-based coffee. In an alternate mode, a grain-type instant coffee composition can be prepared using a mixed bed of soluble grain and coffee solids. Moreover, the core of grain beverage compositions can comprise mixtures of coffee and roasted grain aroma/flavor components. As can be seen from the foregoing, the process of this invention provides a convenient means for manufactur- ing water-dispersible compositions for use as instant foods, instant beverages, or the like, comprising atomizing an aroma concentrate, a flavor concentrate, or a mixed aroma/flavor concentrate commensurate with said food, beverage, or the like1 as droplets into a fluidized bed, said fluidized bed comprising a multiplicity of particles, flakes, or mixtures of particles and flakes, comprising a dried extract of said food, beverage, or the like, whereupon said particles and flakes form aggregates on said droplets; followed by drying said aggregates substantially immediately after their formation. In this fashion are prepared various instant soup (e.g., beef, lamb, pork, mutton, and poultry, especially chicken and turkey), instant beverage, etc., compositions 'which rapidly dissolve in water.

Claims: CLAIMS 1. A process for manufacturing a water-dispersible composition for use as an instant food, instant beverage( or the like, characterized by: (a) atomizing a liquid aroma concentrate, a flavor concentrate, or a mixed aroma/flavor concentrate commensurate with said food, beverage or the like, and having a viscosity of from 5 centipoise to 200,000 centipoise, as droplets into a fluidized bed, the solids in said fluidized bed comprising a multiplicity of particles, or mixtures of particles and flakes, comprising a dried extract of said food, beverage, or the like, at a ratio of roplets;solids of at least 1: :5 by weight, whereupon said particles and flakes form aggregates on said droplets, said aggregates having a moisture content less than 15%; and (b) drying said aggregates substantially immediately after their formation to a moisture level of less than 108 . 2. A process according to Claim 1 characterized by allowing said particles, flakes, or mixtures of particles and flakes to substantially surround and encapsulate said liquid droplets, prior to drying. 3. A process according to Claim 1 or 2 characterized in that said mixture of particles and flakes is at a weight ratio of flakes:particles in the range from 30:70 to 70:30:. 4. A process according to any of Claims I to 3 characterized in that the flakes have diameters in the range of from O.5mm to 12.7mm. 5. A process according to any preceding Claim characterized in that the particles or flakes comprise a dried, watersoluble grain extract. 6. A process according to Claim 5 characterized in that the grain extract is a malted barley extract, 7. A process according to any preceding Claim characterized in that the drying step comprises hot air drying. A < process according to Claim 7 characterized in that the hot air drying step further comprises forced air vibratory drying. 9. A process according to Claim 8 characterized in that the forced air aTibratcry drying is conducted for about one minute at a hot air temperature of from 900C to 1000C. 10. A process according to any preceding Claim characterized in that the aggregates are dried to a moisture level of from 2.5E to 4.5g

Inventors: PFLAUMER, PHILIP FLOYD, WEISMAN, PAUL THOMAS
Applicants: THE PROCTER & GAMBLE COMPANY
Application year: 1979
Main classification: A23L1
IPC codes: A23L1, A23L2, A23F5, A23F3