CA1144814A - Rapidly soluble sweetener - process for its preparation and beverage mix employing it - Google Patents

Rapidly soluble sweetener - process for its preparation and beverage mix employing it

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Publication number
CA1144814A
CA1144814A CA000371123A CA371123A CA1144814A CA 1144814 A CA1144814 A CA 1144814A CA 000371123 A CA000371123 A CA 000371123A CA 371123 A CA371123 A CA 371123A CA 1144814 A CA1144814 A CA 1144814A
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Prior art keywords
dry
less
process according
solution
composition according
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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CA000371123A
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French (fr)
Inventor
Esra Pitchon
Marvin Schulman
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General Foods Corp
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General Foods Corp
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Classifications

    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B50/00Sugar products, e.g. powdered, lump or liquid sugar; Working-up of sugar
    • C13B50/002Addition of chemicals or other foodstuffs
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385Concentrates of non-alcoholic beverages
    • A23L2/39Dry compositions
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/40Effervescence-generating compositions
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • A23L27/33Artificial sweetening agents containing sugars or derivatives

Abstract

RAPIDLY-SOLUBLE SWEETENER, PROCESS FOR ITS PREPARATION AND BEVERAGE MIX EMPLOYING IT ABSTRACT The present invention provides a rapidly-soluble sweetener, a process for preparing it, and improved dry beverage mixes employing it. The composition preferably comprises from 15 to 65% fructose, from 15 to 30% of low dextrose equiva-lence dextrinized starch, and from 30 to 65% sucrose, on a dry solids basis. By preparing it with a density of 0.4 or less, solubility is greatly en-hanced over prior art sweeteners, especially sucrose. Because of the improved solubility, carbonation is not lost by requiring stirring of a sweetener when preparing a beverage from a dry carbonated beverage mix.

Description

DESCXIPTION

RAPIDLY-SOLUBLE SWEETENER~ PROCESS FOR
ITS PRE~ARATION AND BEVERAGE MIX ~MPLOYING IT

Technical Field _ 05The present invention relates to the field of sweeteners, and more particularly to a rapidly-soluble sweetener, especially one suitable for dry beverage mixes.
Dry mixes for beverages, puddings, gelatin desserts, whipped toppings, frostin~s, icings, ice cream, and the like must be free-flowing to provide satisfactory dispensing, accura~e measuring and uniform mixing. Many sweeteners form clumps, which not only adversely af~ec~ these functions, but make dissolving them more dif~icult. Other sweeteners, such a~ sucrose, which is the typical sweetener used in dry mixes, are ordinarily difficultly soluble at concentrations required. For example, when whipped topping mixes contain granular sucrose, a slight graininess sometimes remains even after vigoruus mixing. And, in beverage mixes, vigorous mixing is usually required to obtain complete dissolution o~
granular sucrose. This can be a mild annoyance to a ho~, thirsty individual trying to prepare a single serving of a beverage ~rom a dry mix, especially in -.,, ~ ~ . . . ;

ice water. More critically, however, the need for vigorous stirring can seriously detract from the ability of a dry carbonated beverage mix to satis-factorily perform. The degree of stirring necessary 05 to adequately dissolve sucrose in cold water can seriously dissipate beverage carbonatian.
There is a need for, and ~he present invention provides, a carbohydrate-based ~weetener which is dry and free flowing, and rapidly and completely soluble in water or a~ueous solution in amounts required for sweetness.
Back~round Art The prior art has provided a number of pro-cesses for drying sugar solutions which comprise first forming a massecuite slurry composed of micro-crystals of sucrose. Representative of variations on the massecuite approach is U.S. Patent 3,582,3~9 which discloses that a granular free-flowing and rapidly soluble product is obtained by granule enlargement with a massecuite slurry. The masse-cuite can contain dextrose or a high dextrose equi-valence starch hydrolysate in addition to the sucrose. In U.S. Patent 3,619,293 ~here is a process for forming free-flowing, rapidly dissol-vable crystalline sucrose products by spraying anddrying a massecuite, and then aging the resulting aggregates. The product can contain various additives such as other sweeteners, such as sugars. In U.S.
Patent 3,619,294, dried massecuite aggregated micro-crystalline sugar granules are employed as a means tocombine crystalline sugar with additives. Where the sugar i5 a relatively non-sweet sugar such as dex-trose, a sweeter sugar such as ~ructose can be impregnated into the granules. However, these : . .

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products will sink rapidly in water and require considerable agitation to dissolve. , In U.S. Patent 3,271,194, an alternative to the massecuite approach is disclosed. Therein a sugar 05 solution and solid sugar are simultaneously atom-ized such that they undergo mixing. The product is dried to a density of above 50 grams per 100 cubic centimeters, but needs considerable agitation for dissolution.
In U.S. Patent 3,836l396, a ta~le sugar substi tute which is less cariogenic than sucrose is dis-closed. This product is a physical admi~ture of scucrose and fructose and~or maltose. Again, how-ever, the product will sink rapidly in water and requires considerable stirring to dissolve.
European Pa~ent Application Publication No.
0,000,077, filed Dec. 12, 1978 and claiming priority in ~.S Patent Application No. 803,337, iled June 3, 1977~ specifically addresses the use of sweeteners in dry mixes for carbonated beverages and discloses the use of essentially pure crystalline fructose.
~t is disclosed that the dry beverage mix, contain~
ing th~ fructose, carbonates more rapidly than when sucrose is e~ployed; however~ the fructose-contain-ing be~erage mix will sink when added to water andrequires considerable mlxing to dissolve.
Along this same line, U.S. Patent 3,gS6,00~
describes the preparation o~ product by spray drying a fructose solution. Here, fructose solutions are dried in the presence of separately introduced recycled products. Here again the products sink and cause solubi~ity difficu~ties.

fa Disclosure of Invention In accordance with the present invention, there are provided a dry, rapidly-soluble sweetener compo-sition, a process for preparing the sweetener, and a 05 dry beverage mix i~proved by it. The sweetener composition has a density o less than 0.40 grams per cubic centimeter and comprises a codried inti-mate mixture of from 5 to 85% fructose, from 5 to 60% dextrinized starch having a dextrose equivalence of less than about 15, and from 0 to 80% sucrose, all percentages being based on the dry weight of the composition. The process of the invention is useful for preparing products of this type and comprises:
(a) preparing an aqueous solution comprising, on a dry solids basis, the materials indicated above, (b) dispersing a gas into the solu~ion; and (c) drying the solu~ion under conditions effective to produce a porous product having a density of less than 0.40 grams per cubic centimeter. The improved dry bever~
age mix comprises 1avor, acidulent, coloring and a rapidly-soluble sweetener as defined in claim 1.
Best Mode for Carrying Out the Invention The sweetener compositions of the present -invention have a wide range of utilities, including all of the applica~ions in dry food mixes for which sucrose is normally employed. The following descrip-tion will~ however, focus on the preparation of the sweetener for use in a dry mi~ for forming a beverage particularly a carbonated beverage.
The product for use in a beverage mix should be free-flowing and dry, to facilitate accurate metering and dispensing in automatic packaging equipment. The formation of clumps during storage, either before or after packaging, can result in difficulties. The product should, ~herefore, also be relatively non-hygroscopic. It should, however, have a sweetness about the same as sucrose, because of the widespread familiarity with the relative 05 sweetness of sucrose. Most importantly, the product should be rapidly soluble and require little or no agitation in the amounts required to obtain suitable sweetness.
It is an advantage of the products of the present invention that they float, at least momen-tarily, on the surface of water or aqueous liquid prior to submerging, and then dissolve completely, or nearly so, with no agitation. The preferred products of the invention will float momentarily on the surface of water in a drinking glass, and then completely dissolve almost immediatley upon sub-merging. These preferred products, thus, do not require any agitation to assure their complet.e solution.
The sweetener composition will contain at least 5% and as much as 85% fructose, depending on the desired balance to be struc~ between its various beneficial properties. The more preferred products, especially for use in beverages, will contain from 10 ~o ~5% fructose, and those presently considered most preferred will contain from 15 to 65%. The fructose is impartant for a number of functions, including its intense sweetness and its good solu-bilit~. Fructose from any source can be employed.
The fructose can be employed in its pure form or in mixture with up to 30% non-fructose carbohydrates, such as those residual carbohydrates remaining from the conversion of starches fro~ wheat, corn, potato, and cassava. High fruc~ose s~arch syrup is meant to define those products of the enzymatic conversion of starches to a mixture of saccharides wherein fructose 05 predomi~ates and is preferably present in amounts of above 80% and, most preferably, about ~0% or above, based on the weight of the solids. Particularly preferred are those syrups prepared from corn.
Represe~tative of these are the syrups available under the trademarks: Isomerose from Clinton Corn Processing Co., Corn Sweet from ADM Company and Isosweet from Staley Manufacturing Go. These syrups typically have moisture contents within the range of from 10 to 25~/o~ which is useful in forming the solution with ~he dextrinized starch 5 and preferabl~
also sucrose, in obtaining the codried intimate mixture.
The dextrinized starch employed according to the present invention will have a relatively low dextrose equivalence (DE) to maintain an overall low hygroscopicity for the composition and make it a be~ter carrier for the highly hygroscopic fruetose.
Typically, the DE should be less than about 15 and will preferably be within the range of from about 0.5 to 10. The dextrinized starch will be employed, on a dry solids weight basis, at a level of from 5%
to 60%, and preferably at a level of from 10% to 50%. Most preferably, the dextrinized starch will be present at a level within the range of from 15%
to 30% ba~ed on the total weight of the composition.
There is no known criticality in the manner of preparing the dextrinized starch, and it is believed that material from any of the known procedures can be employed. Representative of the sui~able commer-cially available dextrinized starches are those sold under the Morex trademark by Corn Products Corp, and under the Frodex trademark by American Naize Pro-05 duc~s Corp.
The presence of sucrose is not essential,according to the broadest aspects of the invention;
however, it can be present at levels of up to 80%.
It is, in fact, preferred to employ sucrose for its contribution to sweetness and because it is believed to accentuate sweetness. According to the pre-ferred embodiments, then, sucrose is employed at a level o~ from 15% to 70% and is most preferably employed at a level within the range of from 30% to 50%, all percentages based on the dry weight of the total composition. It is an unexpected advantage of the present invention that the solubility of sucrose can be greatly enhanced, even when present in major amounts, and in the presence of a low ~E dextrinized st.~rch. The products of the invention employing sucrose are further advant~geously unique because they can provide essentially the same sweetness per unit weight as sucrose, but do so in a product with greatly improved solubility.
It is presently believed important to have the components of the composition present as a codried intimate mixture having a density of less than 0.40 grams per cubic centimeter. The preferred products will have densities less than 0.30 grams per cubic centimeter, and most preferably less than 0.25 grams per cubic cen~imeter. There is no known lower limit on this density range from an effec~iveness stand-point; however, products containin~ less than 0.05 . .

grams of solids per cubic centimeter may cause problems in handling, and densities of less ~han Q.10 grams of solids per cubic centimeter will be very cos~ly to produce and handle.
05 The preferred compositions of the present invention appear to-tally amorphous when viewed with the unaided eye. It is believed that the composi-tions do contain crystals, but that the crystals are so small tha~ they are not distinguishable as such and do not adversely affect the solubility o~ the composition. The mos~ preferred compositions will be present as what may be referred to as "solid solutions." This term is meant to define ~n inti-mate associatio~ of the components of the composi-tion in the solid form in units too small to be distinguished by optical microscope. Thus, this term defines a completely homogeneous mixture of the components in the solid form as they would appear a~ter codrying an aqueous solution under conditions effective to maintain crystal formation at an abso lute minimum, preferably prevent any significant crystal formation.
The products of the invention can be ground and sized as desired. It is an advantage of the inven-tion that the solubility of the product remainsexcellent without close control o~ the particle size, which traditionally has been a key factor in the rate of solubility. It is believed that the formulation of the invention, together with its . .

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light, porous nature, provi~es th~ rapid, complete solubility obtained by the products of the invention Preferred products are, however, ground to obtain a desirable free-flowing property and will preferably 05 be screened such that 35% pa~s though an 8 mesh U~S.
Standard Sieve and are retained on a 100 mesh U.S.
Standard Sieve (having approximately a 0.15 mm opening). The most preferred products will be sized to pass through a 20 mesh seive (having approx-imately a 0.84 mm opening) and be retained on a 100 mesh sieve (having approximately a 0.15 mm opening~
with an average particle size of 400 microns.
The process, according to the invention, forpreparing the rapidly-soluble sweetener composition comprises, in its broad aspects: preparing an aqueous solution with the solids as defined above, dispersing a gas into the solu~ion, and then drying the solution under condi~ions effective to product a porous product having a density of less than 0.4 grams per cubic centimeter~ There is no known criticality for the specific equipment employed to carry out this process and any of the known pro-cedures of foam drying, spray drying, freeze drying, tray drying, and the like, which can be perormed under conditions capable of incorporating the de-sired amount of void space in the product to obtain the desired densities, while drying the product to a moisture content effective to provide a free 10wing product, can be employed.
It has been ~ound, experimentally, that pro-ducts produced by dryers of the type described in U.S. Patent 4,116,756, provide highly sa~isfactory results with good reproducibility.

,., ~ ~.

:: :

It will be understood that with the type of equipment o U.S.
Patent 4,116,756, as with all others, it is essential to disperse a gas into the solution prior to drying the solution.
The apparatus described in U.S. Patent 4,116,756 com-prises three basic processing stages within a single housing.
In the first stage, the solution to be dried is conducted to a spray nozzle under superatmospheric pressure, sprayed through drying air~ and collected on a belt. The belt is then passed to the second stage, wherein drying air from the first and third stages is passed through the product on the belt. In the third stage, cooling air is passed through the product on the belt.
This process works especially well according to the present in-vention, where a gas is injected into the solution at a super-atmospheric pressure of at least about 50 psig (approximately 3.5 Kg/cm ), preferably about 100 psig (approximately 7 Kg/cm ) greater than the superatmospheric pressure under which the solution is conducted to the spray nozzle. By dispersing the air in the solution in this manner, and discharging the spray from the nozzle in droplets, rapid drying into a very desirable product is obtained. This is in part due to the expansion of the drop-lets upon discharge. This increases the surface area of the solution to improve not only drying but also subsequent dissolution in water. Moreover, the voids created in this manner decrease the density of the product and enable it to float on the sur-face of water momentarily before it becomes moistened and sub-merges. Upon submersion, the products will almost instantly dissolve.

.~ .
, The solution as discharged can be at any solids concentration effective under the prQcessing condi-tions to provide a product having the desired charac-teristics. Typically, solids contents should be at 05 least 10% to provide efficient drying and less than 80% to provide a workable viscosity. Preferred solids contents will be within the range of from 45%
to 70%.
From discharge at the spray nozzle, the drop-lets are contacted with drying air h~ving a temper-ature within the range of ~rom 180 to 220F (approx-imately 82 to 104C). The solution is contacted, typically, for from 1 to 5 seconds during its ~all through the drying air and collects as a mat on a porous belt which continuously moves through the fi~st drying chamber. At this point the material will have a moisture con~ent within the range of from 75% to 95%, preferably from 80% to 90%. From the first chamber, the ma~ is passed to a second chamber where further air, preferably having a temperature within the range of from 130 to 170F
(approximately 54 to 77C) and a relative humidity with the range of from 10% to 40%, is passed through the mat. The moisture content during this stage in processing will be reduced to near its final level of less than 3%, and preferably less than 2%.
In a third stage, cool dry air is passed through the product on the mat to reduce its temper-ature to a level effective for further processing such as grinding, sizing, mixing with other mat-erials if desired, and packaging. The air desirably has a reduced relative humidity, preferably of from 10% to 30%, and a reduced temperature, preferably of from 60 to 90F (approximately 16 to 32QC).

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More conventional spray drying equipment can also be employed to effect drying. Typical of the dryers is a spray tower manufac-tured by Proctor and Schwartz Company of Philadelphia Pa. For operating 05 a dryer of this type, the solution is preferably fed to a spray nozzle under a pressure of 120 psig (approximately 8 Kg/cm2) and air or other gas is injected into the feed stream at 1400 psig (approxi-mately 98 Kg/cm~). In spray towers of this type having inner and outer cones, the inner cone is preferably cooled, such as with ambient air to prevent the product from adhering to the tower walls. The solution is contacted with drying air at an inlet temperature of 220F (approximately 104C) and an outlet temperature of 150F (approximately 66C).
Freeze drying under conventional conditions can also be employed. Typical of ~.he drying equipment is Stokes*Shelf Freeze Dryer. During freeze drying, the product is subjected to a vacuum, and the air which is dispersed in ~he solution due to its normal solubility in water and during preparation of the solution will cause expansion of the product during drying. Also, the solution of water vapor by the ~5 drying procedure will cause further expansion.
Thus, injection of gas into the solution just before drying is not essential in free~e drying and, in fact, does not appear to markedly affect the end product. This loosely dispersed air, unlike in spray drying, is not necessary to expand the product and is rapidly lost from the product in the early stages of vacuum application, or even before this.
Where desired, however, air or other gas can be injected.

* Trade Mark . .

- . . , ~ . , .
. . - , . , The sweetener composition o the invention is ideal for the preparation of dry beverage mixes of the type which comprise flavor, acidulent, color and sweetener; and the rapidly soluble sweetener of the 05 present invention provides improved dry beverage mixes of ~his ~ype because of its improved solu-bility which makes it possible to enjoy the beverage more rapidly with less poten~ially messy mixing.
The formulation of beverage mixes of this type are well ~nown and are exemplified for example in U~S. Patent 4,001,448 to T. Finucane, The colors, flavors, acidulents and other ingredients can be employed in a beverage mix improved by the sweetener of this invention.
The advantages of ~he rapidly-soluble sweetener become especially pronounced when used in dry bev-erage mixes containing a carbonating agent or for use with a carbonat~ng agent in addi~ion ~o the color, flavor and acidulent. Because the sweetener is so rapidly soluble, the beverage does not have to be vigorously agitated to dissolve the sweetener.
This can be a distinct advantage when compared to prior art compositions containing granular sucrose, where the stirring necessary to dissolve the sucrose would partially dissipate the carbon dioxide.
The carbonating agent can comprise a chemical agent, such as calcium carbon~te, alone or with another carbonating agent, such as sodium or po-tassium carbonates or bicarbonates. Or any of theother prior art, chemical carbonating agents can be employed. The carbonation source disclosed by Stahl in U.S. Patent 3,965,273 is particularly suitable, with the rapidly-soluble sweetener of the present ~, .
~, .. ) ~L~

invention ~orming the carbohydrate matrix holding the calcium carbonate particles. Thus, the calcium carbonate can be encap-sulated according to the Stahl teachings, using the rapidly soluble sweetener as the matrix material.
Alternatively, the carbonating agent can be a molecular sieve device having carbon dioxide adsorbed therein. Among the suitable devices are those comprising activated charcoal and zeolites. U.S. Patents 3,930,053, 4,051,268 and 3,983,251, relates to the preparation, composition and use of molecular sieve carbonating devices and the beverage mixes with and in which they are used. The decreased need for agitation afforded by the sweeteners of the present invention improves the performance of all dry carbonated beverage mixes by decreasing the loss of carbonation due to stirring.
The following examples are presented for the purpose of further illustrating and explaining the present invention and are not to be taken as limiting in any regard. Unless other-wise indicated, all parts and percentages are by weight.

EXAMPLE I

This example describes a preferred embodiment oE the invention wherein an aqueous solution of 60 parts sucrose, 20 parts Isomerose 900 high fructose corn syrup, and 20 parts Morex 1918 lODE dextrin, and containing 70% total solids is dried on a DEC Damrow Company Model F500 Filtermat* dryerof the type shown in said U.S. Pat~nt ~,116,756. The * Trade Mark Isomerose 900 contains 90% fructose on a dry solids basis; thus, the amount of fructose in the solution is 18% on a dry solids weight basis.
The solution is fed to one SX-60/21 spray 05 nozzle manufactured by Spraying System Corp., at a temperature of 120F, a pressure of 1500 psig (approximately 105 Kg~cm2), and at a rate of 300 pounds (approxima~ely 136 Kg) per hour. Air is supplied to the first chamber at a t~mperature of 210F and a rate of 2000 cubic eet (approximately 57 cubic meters~ per minute. The air at the outlet from the chamber is cooled by the drying prQCeSS to about 150F ~approximately 66C). Prior to dis-charge from the nozzles, air under ~ pressure o 1700 psig ( approximately 120 Kg/cm2) is charged into the line carrying the solu~ion to disperse it within the solution. The solution is discharged into the drying air in minute droplets which expand and lose moisture as they decend onto a porous belt and form 20 a mat. The ma~erial on the mat has a moisture content of about 85%, never actually measured, as it is removed from the first stage. In a second stage, air at a temperature of about 165F (approximately 74~C) and a relative humidity of about 20% is passed th~ough the product on the belt at a rate of about 500 cubic feet (approximately 14 cubic meters) per minute. Upon exiting the second stage, the moisture content of the product in the mat is at about the flnal l~vel. The third stage cooling chamber is not employed and the product is allowed to cool to ambient. The matted product, which appears amor-phous, is ground by passing it through a 20 mesh U.S. Standard sieve. It is found to have a density - 16 ~
of 0.260 grams per cubic centimeter, as measured by ~he following procedure: Product flows through a funnel into a measure cup. Density is equal to the net weight of a leveled cup over volume. Its mois-05 ture content is found to be 1.06%, as measured bythe following procedure: vacu~m oven for 24 hours at 26 inches Hg and 140F (approxima~ely 660 ~m Hg and 60C~. The product is tested for solubility by dispersing in 60F (approximately 16C) water with-out stirring. It is found ~o be excellent, ra~ing a10 on a scale of 0 to 10 9 with 10 being the highest.
Example II
This example describes the preparation of the sweetener of the invention by freeze drying instead 15 o~ the process of Example I.
According to this example, a solution identical with that of Example I, except that the solids content i~ reduced to 10%, is prepared and freeze dried, using a Stokes Freeze Drier. The solution is ~irst frazen to -110F (approximately -79C), then is placed under vacuum, and is then lyophilized at a plate temperature of 120~F (approximately 49C) at an absolute pressure of 3~0 microns. The product is found to have a moisture content of 1.38% ancl a density of 0.267 grams per cubic centimeter, when measured as in Example I. The produet appears slightly crystalline and dissolves rapidly J rating an 8 when tested as in Example I.
Exam~le III
The procedure of Example II is repeated, but this time employing a s~lids content of 70% in the starting solution.
The product appears sli~htly less crystalline than the produc~ of Example II, and has a density of B~4 . - 17 -0.373 grams per cubic centimeter, a moisture content of 1.78%1 and a solubility rating of 4J all measured as in Example I.
Example IV
05 This example repeats Example III but employs a starting solution with a solids content of 30% and includes the step of injecting carbon dioxide into the solution which is then sprayed by a nozzle on~o a tray prior to freezing. The product appears sligh~ly less crystalline than that of Example II;
and has a density of 0.317 grams per cubic centi-meter, a moisture content of 1.98%, and a solubility rating o~ 4, all measured as in Example I.
Example V
This example repeats the procedure o~ Example IV, but employs a starting solution with a solids content of 50%.~ Again, CO2 was injected into the solution prior to freezing. The product appears slightly less crystalline than that of Example II, and has a density of 0.359 grams per cubic centi-meter, a moisture conten~ of 2.05%, and solubility rating of 5, all measured as in Example I.
Example VI
This example repeats the procedure of Example III, but this time a Votator*type scraped surface heat exchanger is used to cool the starting solution to a temperature of OaF (approximately -18C) as air is fed into the solution prior to freeze drying.
The freeze dried product appears slightly less crystalline than that of Example II; and has a density of 0.369 grams per cubic centimeter, a moisture content of 1.27%, and ~ solubility rating of 5, all measured as in Example I.
* Trade Mark .

Example VII
This example repeats the procedure of Ex~mple VI, but this time employs a solids content of 80% in the starting solution. The resulting product 05 appears as crystalline as that of Example VI; and has a density o~ 0.256 grams per cubic centimeter, a moisture content of 1.97%, and a solubility rating of 5, all measured as in Example I.
Example VIII
10The procedure of Example II is repeated, but this time not employing a composition of ~he inven-tion but using only sucrose in an aqueous solution with a solids~ content of 50%. Although the density of the product is highly crystaline and has a solu-bility rating of 0, all measured as in Example ~.
~xample_IX
This example illustra.tes an alternative method of spray drying a composition i~entical with that of Example V.
20Here a doubls cone spray drier is fed the composition at a feed rate of 200 pounds (approxi-mately 91 Rg) per hour under a pressure of 1100 psig (approximately 77 Kg/cm2). Air was injected at 1200 psig (approximately 84 Kg/cm2) into the solution prior to discharge from a Spraying System Corp. SX
high pressure nozzle having a n~mber 60 orifice and a number 21 spinner. The inlet air temperature is
2.03F (approximately 95C) and the outlet tempera-ture i.5 153F (approximately 67C). Product collect-ed from the tower with an air cooled inner cone had a density of 0.260, a moisture content of 3.3%, and a solubility rating of 10. All o~ these tests are conducted as in Exmample I.

Example X
Formulation consisting of 53 parts sugar, 18 parts Isomerose. 900, 18 parts Morex 1918, and 11 parts of carbonates (sodium bicarbonate, potassium 05 carbonate~ calcium carbonate) at a solid concentra-tion of 70% was dried at condi~ions similar to Example I. Separately a ormulation consisting of 42% sugar, 14% Isomerose 900, 33% Morex 191~, and 11% citric acid at solids concentration of 70% was also spray dried under conditions similar to Example I. The two dried produc~s were com~ined at an approximate 50/50 ratio and provided an instantly soluble-beverage with carbon~tion.
Example XI
This example repeats the procedure of ~xample IX, but this time employs a ~eed solution cont~ining 70% solids and varies certain of the drying con-ditions to produce a series of products.
The inner cone of the spray drier is cooled with air and the drier is operated under the follow-ing canditions to produce products having the follow-ing properties:

Run A B C D
Inlet temp (F) 200 200 203 200 Outlet Temp ~F) 155 155 153 :L65 Nozzle Pressure (psig) 1500 900 1100 925 C2 Injection 1600 1000 1200 1000 Pressure (psig) Product Moisture ~%) 1.3 1.3 3.3 3.2 Product Density 0.2420.242 0.260 0.255 (gm/cc) ; Solubility rati~g 10 10 10 10 An instantly soluble dry beverage mix was obtained by gentle dry admixing 99.32 parts of the dry sweetener product of ~his invention, 0.3 parts 05 of an instant commercial citrus flavor preparation, O.3 parts of a commercially available fine powdered acidulant and 0.08 part~ of a commercially available fine powdered buffer.
Nine hundred milliliters of ice cold water at 4C were placed in a pressure-proof container. On basis of 1 quart final beverage preparation, 96 grams of the above dry beverage mix are used. The instantly soluble dry beverage mix comprising the instantly soluble dry sweetener preparation which is the object of this invention were added into the water and the mixture stirred only very slightly with a long handled spoon. The entire m:ix was practically immediately completely dissolved.
Zeolite ag~lomerated disc shaped bodies similar to those described by Sherman et al, U.S. Patent 4,123,390 Exam~le I (A) charged with carbon dioxide were placed into the beverage and the container was promptly hermetically closed.
Desorbing of carbon dioxide from the adsorbent and gas bubbling through the beverage crea~ed v:io-lent turbulence in the beverage.
Following a ~ive-minute preparation period, pressure was released and container opened.

-A completely clear and transparent, pleasantly tasting refreshing carbonated beverage was obtained having carbonation of 3.50 volumes, (i.e. 3.50 cc per ml of beverage solution measured at standard 0~ tempera~ure and pressure. No haziness was evident and no undissolved residue could be found.
The above description is for the purpose of teaching the person skilled in ~he .art how to prac-tice the present invention. This descrip~ion is not 1~ intended to detail all o the obvious modifications and variations of the invention which will become apparent ~pon reading. However~ applicants do intend to include all such obvious modifications and variations within the scope of their invention which lS is defined by the following claims.

Claims (32)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A dry, rapidly soluble sweetener composition sprayed under superatmospheric pressure and dried, having a den-sity of less than 0.40 grams per cubic centimeter and comprising a codried intimate mixture of from 15 to 65% fructose, from 15 to 30% dextrinized starch having a dextrose equivalent of less than 15, and from 30 to 65% sucrose, all percentages being based on the dry weight of the total composition.
2. A composition according to claim 1, wherein the fructose is comprised of high fructose corn syrup solids.
3. A composition according to claim 1 wherein the components are present as a solid solution.
4. A composition according to claim 1 which is es-sentially amorphous.
5. A composition according to claim 1, wherein the moisture content is less than 3%.
6. A composition according to claim 5, wherein the moisture content is less than 2%.
7. A composition according to claim 1, wherein 95%
passes through an 8 mesh U.S. Standard sieve and is retained on a 100 mesh U.S. Standard sieve.
8. A composition according to claim 1, wherein the dextrinized starch has a dextrose equivalence within the range of from 0.5 to 10.
9. A composition according to claim 1, which has a density of less than 0.30 grams per cubic centimeter.
10. A composition according to claim 9, wherein the dextrinized starch has a dextrose equivalence within the range of from 0.5 to 10.
11. A composition according to claim 10, wherein the fructose is comprised of high fructose corn syrup solids.
12. A composition according to claim 11, wherein 95%
passes through an 8 mesh U.S. Standard sieve and is retained on a 100 mesh U.S. Standard sieve.
13. A composition according to claim 12, which has a density of less than 0.25 grams per cubic centimeter.
14. A dry beverage mix comprising flavor, acidulent coloring and a rapidly-soluble sweetener as defined in claim 1.
15. A dry beverage mix as defined in claim 14, which further comprises a carbonating agent.
16. A dry beverage mix according to claim 15, wherein said carbonating agent comprises calcium carbonate.
17. A dry beverage mix according to claim 16 wherein said carbonating agent comprises a molecular sieve having carbon dioxide adsorbed thereon.
18. A dry beverage mix according to claim 17 wherein the molecular sieve comprises activated charcoal.
19. A dry beverage mix according to claim 17 wherein the molecular sieve comprises a zeolite.
20. A process for preparing a dry, rapidly-soluble sweetener composition which comprises (a) preparing an aqueous solution comprising, on A dry solids basis, from 15 to 65% fruc-tose, from 15 to 30% of a dextrinized starch having a dextrose equivalence of less than about 15, and from 15 to 65% sucrose;
(b) dispersing a gas into the solution at superatmospheric pres-sure of at least about 50 psig; and (c) drying the solution under conditions effective to retain a sufficient amount of the gas therein to produce a porous product having a density of less than 0.40 grams per cubic centimeter.
21. A process according to claim 20, wherein the solu-tion is conducted to a spray nozzle under superatmospheric pres-sure and said gas is injected into the solution at a pressure of at least about 100 psig greater than the pressure of the solution.
22. A process according to claim 21, wherein the solu-tion is discharged from said spray nozzle in droplets which ex-pand upon discharge into a stream of drying air.
23. A process according to claim 22 wherein the drop-lets are partially dried by passage through drying air, are col-lected on a continuously moving porous belt to form a mat, and drying air is passed through the mat to dry the composition to a moisture content of less than 3% by weight.
24. A process according to claim 23, wherein the dried composition is ground.
25. A process according to claim 22, wherein the drying air has a temperature of within the range of from about 190°F.
to 230°F. initially upon contact with the solution as it is dis-charged from the spray nozzles.
26. A process according to claim 20, wherein the dex-trinized starch has a dextrose equivalence within the range of from 0.5 to 10.
27. A process according to claim 20, wherein the fruc-tose is comprised of high fructose corn syrup solids.
28. A process according to claim 20, wherein the dry-ing is conducted under conditions effective to retain a sufficient amount of said gas therein to produce a product having a density of less than 0.30 grams per cubic centimeter.
29. A process according to claim 20, wherein the solu-tion is frozen and then dried by sublimation under vacuum.
30. A process according to claim 20, wherein the solu-tion is formed into a stable foam prior to drying.
31. A process according to claim 20, wherein the solu-tion has a solids content within the range of from 10 to 80% prior to drying.
32. A process according to claim 30, wherein the solu-tion has a solids content within the range of from 45 to 70% prior to drying.
CA000371123A 1980-03-17 1981-02-18 Rapidly soluble sweetener - process for its preparation and beverage mix employing it Expired CA1144814A (en)

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US06/130,941 US4303684A (en) 1980-03-17 1980-03-17 Rapidly-soluble sweetener, process for its preparation and beverage mix employing it
AU75231/81A AU7523181A (en) 1980-03-17 1981-09-15 Rapidly soluble sweetener

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US4303684A (en) 1981-12-01
EP0036738B1 (en) 1984-05-30
ATE7647T1 (en) 1984-06-15
AU7523181A (en) 1983-03-24
DE3163829D1 (en) 1984-07-05
EP0036738A1 (en) 1981-09-30

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