CA2417958A1 - Starch products having hot or cold water dispersibility and hot or cold swelling viscosity - Google Patents

Abstract

Physically modified starch products aa-e prepared using pressure and heat such as by extruding starting material starch which optionally can be admixed with gums and/or surfactants.
The properties of the products can be adjusted by varying the moisture content of the materials in the extruder and the temperature and pressure at a die plate provided at the discharge end of the extruder. The screw elements in the extruder are selected with the goal of using enough mixing elements at the discharge end to keep the pressure in the extruder barrel as high as possible over a short distance. The physically modified starch products are made up of partially to fully cooked starch and some raw starch particles. They are highly dispersible in cold or hot water with hot or cold swelling viscosity.

Description

Attorney Docket No. 3646/9509 STARCH PRODUCTS HAVING HOT OR COLD WATER
DISp~SIBILITy AND HOT OR COLD SWELLING VISCOSITY
C~ O~ I ION
l0 Field of the Invention The present invention has to do with dispersible starch products and particularly relates to physically modified starch products prepared using pressure (shear) and heat such as in an extrusion process. The products of the invention have improved functionality in food applications, particularly in instantiaed hot or cold applications.
Description of RelatQd Art Starches are widely used in food applications as thickeners or bodying agents. They are unique among carbohydrates in occurring as discrete granules. In modern day food processing and storage applications, however, the properties of granular starch must be modified to withstand certain heat, acid and freeze-thaw conditions. Presently, food processors prefer to avoid chemically modified starches and employ natural products such -as physically modified starches.
when granular starch is heated in excess water above the gelatinization temperature, it undergoes hydration and gelatinizes, forming a viscous solubilized paste. In practice, starch granules require dispersion in cold water before cooking at the time of use.

Pregelatinized starch products have been developed that provide reconstituted pastes when mixed with hot or cold water.
The starch manufacturer hydrates the raw starch and then gelatinizes the starch by such techniques as roll-drying or spray-drying and the like. Unfortunately, the dried pregelatinized starch product does not readily disperse in hot water and agglomerated masses are formed giving lumpy pastes with inconsistent paste viscosities.
Attempts have been made to circumvent the dispersibility problem by inclusion of surfactants with dried pregelatinized starch and somewhat improved dispersibilities were obtained as exemplified in U.S. Pat. Nos. 3,53,8938 3,582,350: 3,443,990 and 4,260,62. The effect of surfactants on starch pastes is also described by E. M. Osman in Starch: Chemistry & Technology, Vol.
II, Chapter VII, pp. 189-191; Whistler & Paschall Eds., Academic Press, N.Y. (1967).
The term "heat-moisture treated starch" is known in the art and is commonly used to refer to a starch which has been subjected to a heat treatment under controlled moisture conditions, the conditions being such that the starch undergoes neither gelatinization (i.e., exhibits no substantial loss of birefringence) or dextrinization. If heat-moisture treated starches are used in hot-water dispersible foodstuffs, dispersion of the mix into boiling Water nevertheless results in formation of lumps and agglomerated or coated masses by surface gelatinization wherein a coating barrier forms on the starch preventing further hydration.

2 A hot or boiling water dispersible starch product that consistently provides a uniform paste having no lumps or agglomerated masses associated therewith is described in U. S.
Patent No. 4,491,483.
The combination of starch and gums or starch, gums and emulsifiers iS generally known (see U.S. Pat.. NOS. 3~917,875~
4,140,566; 4,081,567: 4,105,461: 4,119,564; 4,120,986s 4,140,808 and 4,192,900). The gums are used as thickeners or. stabilizers in these formulations. Nevertheless, food formulators prefer to use as much starch as possible in these products due t~ the high cost of gums .
Methods of modifying starch and blends of starch and gums using extrusion are known. U. S. Patent No. 4,859,484 describes a method of processing starch and gum blinds wherein the starch and gum are separately hydrated, intimately commingled and extruded. The method requires water in the amount of 70-200%
based on starch weight. Two other U. S. patents, Nos. 5,208,061 and 5,275,774, describe extrusion methods for making starch products. The use of extrusion to modify starch also has been described by Shaw S. Wang in "Gelatinization and Melting of Starch and Tribochemistry in Extrusion", Starch/Starke 45 (1993) ~dr.ll, pp 388-390.
Applicants have now discovered an improved method of physically modifying starches and mixtures of starches and other materials using pressure and heat, such as by extrusion under specified conditions of moisture, temperature and pressure. The physically modified products of the improved method can be made

3 . . CA 02417958 2003-02-20 for high dispersibility in hot or cold liquids and do not form agglomerated masses.
S Y ~F THE I I~N
Physically modified starch products haying improved functionality in food applications are prepared by extruding starch or mixtures of starch and , starch and surfactant, or starch, gum and surfactant. ~n unmodified starch from one farinaceous material or combinations of unmodified starches from different farinaceous materials and/or a modified starch or 30 starches (such as chemically, genetically or physically modified starches) can be employed as the starting material starch. When gum is mixed with the starting material starch, one or a combination of gums can be used. ~ surfactant which can be one or a combination of surfactants is added to the starting material starch or starch/gum mixture when a modified starch-surfactant product is desired. The term starting materials as it is used herein means starting material starch, or a mixture of starting material starch and gum, or a mixture of starting material starch, gum and surfactant, or a mixture of starting material starch and surfactant.
The properties of the products of the invention are manipulated by controlling the conditions of extrusion such as the moisture content of the material in the extruder and the die plate temperature and pressure of the extruder.
Known equipment for modifying starches other than extruders can be employed to make the products of the invention and such equipment includes spray dryers, roll dryers, compacting rolls, mills, explosion puffers and other means which allow the operator to control the pressure (or shear), temperature and moisture of the starting materials so that the desired product properties can be obtained.
When mixtures of more than one starch, or starting material starch With other components such as gum and/or surfactant, are employed, the mixtures can be prepared partially or completely before they are added to the extruder or they can,be prepared by mixing in the extruder itself. The terms mixture, admixture, to blend and the like are used interchangeably in this specification.
The products can be used in many applications calling for modified starch, including food applications such as dry gravy/sauce mixes, (i.ee spaghetti sauce, turkey gravy, hollandaise sauce), salad dressings (pourable and spoonable), instantized starch (for home use), pudding mixes, soup and carriers for dough_conditioner, (baking). The products of the invention also exhibit desirable viscoelastic properties (characteristics that are related to desired mouthfeel that are associated with fat mimetic materials).
The extruder is operated with the objective of providing controlled mixing of,starch granules such that the end product is a heterogeneous mass of gelatinized, partially gelatinized and ungelatinized starch granules as indicated by photomicrographs.
The extruder also is operated with the objective of maximizing mechanical energy levels while minimizing thermal energy input.
A screw element configuration for the extruder is selected with the goal of using enough mixing elements at the discharge end to.
keep the pressure in the barrel as high as possible over a short distance. Moisture content of the starting materials is adjusted by adding water prior to introducing the starting materials into the extruder and/or by water injection into a first section of the extruder barrel at or near the inlet for the starting materials. A die, having a variable orifice or a preselected fixed orifice, is used as a means to control the die-plate pressure within a predetermined range. Pressure and temperature 1~ at the die-plate also are a function of the screw configuration and rotational screw speed (revolutions per minute), the rate of feed into the extruder and the composition of the material in the extruder: Temperature is also a function of any cooling or heating added by means ~f a barrel jacket. When the product exits the die orifices) of the extruder, water flashes~off as steam, thus reducing the moisture content of the extrudate.
A characteristic of the process is that it requires minimal external temperature control of the type provided by heating and/or cooling jackets surrounding the extruder barrel and in some cases sufficient heat is provided by shearing within the extruder barrel so that no external heat is needed. The ingredients preferably are added to the extruder at ambient temperatures although pre-heating or pre~cooling of the starting materials and/or added water can be used as a means of achieving desired temperatures within the extruder.
The products of the invention can be dried and/or ground or milled provided that the conditions ~f drying, grinding or r milling are selected so as to avoid further gelatinization and loss of functionality of the product. Accordingly, it is preferable to dry at temperatures of about 120nF or less and employ multiple pass grinding or milling to avoid overheating. Conventional dryers such as belt dryers, tube and pneumatic tube dryers, toroidal dryers and flash dryers can be employed. Conventional grinding or milling equipment also can be employed such as a FITZ (trade-mark) comminuting machine.
The invention also relates to a unique agglomeration procedure which can be used to enhance the dispersibility of the products in hot systems.
All percentages set forth herein are by weight and all ratios are expressed in terms of weight/weight unless otherwise designated. All references to the weight of starch, starting material starch or starting materials herein include the moisture present therein.
BRIEF DESCRIPTION ~F THE DRAWINGS
Fig. 1 is a side view in partial cross-section of an extruder barrel with screws disposed therein.
Fig. 2 is a top view in partial cross-section of an extruder barrel with screws disposed therein.
Fig. 2a illustrates a single orifice die.
Fig. 2b illustrates a multiple orifice die.
Fig. 2c illustrates an adjustable orifice die.
Fig. 3 is a 9 unit 3/4 pitch screw designated as WENGER (trade-mark) 55325-003.

' - CA 02417958 2003-02-20 a Fig. 4 is a 9 unit 3/4 pitch cone screw designated as Wenger 55321°005.
Fig. 5 is a 9 unit full pitch screw designated as Wenger 55357-003.
Fig. 6 is a 6 unit full pitch screw designated as Wenger 55357-103.
Fig. 7 is a 9 unit 1/2 pitch screw designated as Wenger 55326-003.
Fig: 8 is a 6 unit 1/2 pitch screw designated as Wenger l0 55326-103.
Fig. 9 is a triple flight cone screw designated as~Wenger 55387-003.
Fig. 10 is a 4.5 unit 3/4 pitch screw designated as Wenger 55395-003. -Figs. il, 12 and 13 are thick shearlocks designated as Wenger 55324-101, 55324-103 and 55324-105, respectively.
Figs. 14 and 15 are thin shearlocks designated as Wenger 55364-101 and 55364-103, respectively.
Fig. 16 is a photomicrograph of a product of the invention taken with partially crossed polarizing filters at 75X
magnification in an oil media having a refractive index .of 1.604.
Fig. 17 is a photomicrograph of a p~~oduct of the invention taken at 75X magnification in a glycerin and water media.
Fig. 18 is a photomicrograph of a product of the invention taken with partially crossed polarizing filters at 75X
magnification in a glycerin and water media.

Fig. I9 is a photomicrograph of a product of the invention taken with partially crossed polarizing filters at ?5X
magnification in an oil media having a refractive index of 1.604.
Fig. 20 is a photomicrograph of a product of the invention taken at 75X magnification in.a glycerin and water media.
Fig. 21 a photomicrograph of a product of the invention taken with partially crossed polarizing filters at 75X
magnification in a glycerin and water media.
Fag. 22 is a photomicrograph of a commercial pre-gelatinized corn starch taken with partially crossed polarizing filters at 75X magnification in an oil media having a refractive index of 1 . 6 4 0 Fig. 23 is a photomicrograph of a commercial pre-gelatinized corn starch taken at ~5X magnification in a glycerin and water media.
Fig. 24 is a photomicrograph of a coaamercial pre-gelatinized corn starch taken with partially crossed polarizing filters at 75X magnification in a glycerin and water media.
Fig. 25 is a photomicrograph of a commercial, spray-dried, modified starch taken with partially crossed polarizing filters at 75X magnification in an oil media having~a refractive index of 1.604.
Fig. 26 is a photomicrograph of a commercial, spray-dried, modified starch taken at 75X magnification in a glycerin and water media.

Fig. 27 is a photomicrograph of a commercial, spray-dried, modified starch taken with partially crossed polarizing filters at 75X magnification in a glycerin and water media.
DBTIS.II,ED DESCRIPTIOI~T OF TE8 IN~BZfPION
Starches derived from one or a combination of farinaceous materials can be used as starting material starch according to the invention. Any farinaceous material can be used as the source of the starch including corn, waxy corm, wheat, potato, tapioca, manioc, grain sorghum, sago and rice, among others.
l0 Accordingly, the starting material starch can be comprised of one type of unmodified starch, blends of different types of unmodified starch, a modified starch or starches and/or blends of modified and unmodified starches. The starting material starch generally will have a moisture content from about 8% to about 13%.
A gum or a mixture of gums can be employed in combination with the starting material starch and the term gum herein can refer to one gum or a combination of gums. Suitable gums include locust bean gum, xanthan gum, guar gum, gellan gum, prehydrated gum and the like.
When an admixture of starch and,gum is employed, the gum is added in an amount from about 0.05% to about 20%, preferably from about 0.05% to about 10% and most preferably from about 0.5 to about 5% based on starting material starch weight.
At the start-up of the process, when the starting materials are first introduced into an extruder, an excess of added water is used as a diluent to facilitate flow through the extruder.

' CA 02417958 2003-02-20 Typically, the extruder is started with water and then the starting materials are gradually added. As the rate of addition of starting materials is increased, the rate of water addition is decreased until the desired steady state processing conditions are achieved. The water is admixed with the starting materials at or near the inlet of the extruder. As an option, some excess water also can be added to the starting materials before they are introduced into the extruder.
The desired steady state operation (i.e. a steady state continuous extrusion process) according to the invention is achieved at a total moisture content (i.e. all of the materials being processed in the extruder, namely added water plus the moisture content of the starting materials) of from about 18% to about 45%, preferably from about 18% to about 35%, and most preferably from about 20% to about 30% based on starting material starch weight. The moisture content is controlled within this range in order to manipulate the properties of the end product, with lower moisture processing conditions yielding a product having less gelatinization than higher moisture processing conditions.
When starting material starch and a gum are employed as the Starting materlalS, the moisture Content at Steady State operation of the extruder also is controlled within the same ranges as described above and the processing parameters and properties of the end products are manipulated in the same manner as described above.

In the embodiment of the invention wherein a surfactant is employed with a starting material starch or both starting material starch and gum to make up the starting materials of the invention, the surfactant can be made. up of one or a combination of surfactants and they generally are employed in an amount from about 2% to about 50%, and preferably from about 2% to about 35%, based on the weight of starting material starch. Suitable surfactants include food emulsifiers such as glycerides, preferably a mono- or di-glyceride of fatty acid. Exemplary surfactants include glycerol monostearate, sodium stearoyl-2-lactylate, calcium stearoyl-2-lactylate and other alkali metal salt stearoyl-2-lactylates, palmitic or stearic fatty acids, D-glucose 3-stearate, methyl alpha-D-glucoside-G-stearate, sucrose monostearate, sorbitan tetrastearate, thereof, sodium stearoyl fumarate and the like. The moisture content at steady state and the processing parameters and properties of the end product are manipulated in the same manner as described above.
Various types of extruders can be employed according to the invention provided that they can be operated in a manner whereby pressure and temperature conditions within the extruder and the pressure and temperature at the die plate can be controlled.
Single screw or twin screw extruders can be employed but the preferred extruders for most applications are 'the twin screw type because they have better barrel heat transfer and they can achieve better mixing. Suitable extruders have a barrel and a screw element or two screw elements disposed within the bore thereof. The configuration of the screw elements can be varied to modify the operating properties of the extruder and the properties of the products of the invention.
A die plate is provided at the discharge end of the extruder and the size of the orifice or orifices in the die plate are selected to achieve the desired die plate temperature and pressure. The die plate pressure is adjusted' to between about 200 and about 2500 pounds per square inch gauge (abbreviated herein as "psig or p.s.i.g."), preferably from about 500 to about 1600 psig, and the die plate temperature is controlled at from about 140°F to about 285°F, preferably from about 140°F
to about 265°F. It is understood that the die plate temperature may be somewhat lower than the temperature of the extrudate.
A twin screw extruder is illustrated in the drawings wherein Fig. 1 is a side view in partial cross-section of extruder barrel 1 with screw 3a disposed within the bore 4 thereof. The same elements are illustrated in Fig. 2 which is a top view in partial cross-section wherein both screws 3a and 3b are shown. The screws are corotated clockwise by conventional drive means (not shown) so that the starting material starch or starting materials 2~ which are introduced into the extruder inlet 5 are moved to the left and forced toward die plate 6 and through orifice 7 thereof.
The die plate 6 can have one orifice ~ or multiple orifices a as illustrated in the partial perspec~.ive views Figs. 2a and 2b, respectively. Adjustable orifice die plates also can be used wherein.the size of the opening of one or more orifices can be changed, thereby changing the die plate pressure. As the flow rate in the extruder is increased, the size of the orifice is ~. 3 ~

increased to maintain the desired temperature and pressure at the die plate. A single opening adjustable orifice die plate is illustrated in a partial perspective view Fig. 2c wherein adjustment thumb screw 8 is used to change the site of the opening of orifice ~. The mounting bolts 16 disposed near the perimeters of each die plate serve to attach the die plate to the discharge end of the extruder.
Water is introduced into the extruder through inlet 9 and the starting material starch or starting materials are introduced into the extruder through inlet 5. As discussed above, an excess of water is used at the start up of the process followed by a gradual reduction until steady state processing conditions are achieved. At steady state, the moisture content of the material being processed in the extruder is maintained at a relatively constant value, within a desired controlled tolerance, and the die plate temperature and pressure are sa.milarly maintained at relatively constant values.
The screws 3a and 3b are made up of various extruder elements. The extruder elements used to make up the screws which were employed in the working examples of the invention are illustrated in Figs. 315. The screws 3a and 3b shown in Figs. 1 and 2 illustrate a configuration of screw elements affixed on hexagonal shafts l0a and lOb with mixing elements 11 and 12 made up of various combinations ~f the shearlock extruder elements shown in Figs. 11-15 and the conveying elements 13 and 14 are made up of various combinations of the extruder elements shown in Figs. 3, 5-8 and 10. Cone screws 15a and 15b (see also Figs. 4 ' CA 02417958 2003-02-20 and 9) are provided to increase pressure just before the die plate. As discussed above, the screw elements are configured to make screws having suitable mixing elements at the discharge end to keep the pressure in the barrel as high as possible over a short distance.
The products of the invention can be made for high dispersibility in hot or cold liquids and d~ not form agglomerated masses. The characteristics of the product are determined by the starting materials and by the processing 1~ conditions of moisture-content, pressure (shear) at the die plate and temperature at the die plate. The temperature and pressure in the extruder upstream of the die plate may also be controlled to obtain the desired characteristics of the product and such control is achieved by varying the rotational screw~speed, varying the rate of feed into the extruder, and cooling and/or heating using jackets. Accordingly, the processing conditions are selected to obtain a product comprised of gelatinized, partially gelatinized and ungelatinized starch granules in a heterogeneous admixture. The relative amounts of gelatinized, 2o partially gelatinized and ungelatinized material will determine the characteristics of the product with respect to dispersibility and viscosity. Products having a higher degree of gelatinized granules are most easily dispersed in liquids and those with less fully cooked particles will provide higher viscosity.
Photomicrographs of the products of the invention show a range of gelatinization from fully cooked through partially gelatinized to raw granules in a heterogeneous~mixture. It is hypothesized that this range of gelatini2ation provides the unique combination of dispersibility and viscosity which characterize these new products.
The thickening power of starch can be predicted analytically by measuring hydration capacity. The following method was adapted from AACC Method 56-20, available from American Association of Cereal Chemists, 3340 Pilot Knob Road, St. Paul, Minnesota 55127-2097 U.S.A~, by doubling weights and volumes to use a 250 ml. centrifuge tube, and was used to measure hydration l0 capacity of the products of the inventiono 1. Determine sample dry substance (d.s.).
2. Record tare weight of centrifuge tube.
3. Add a 4 gram sample "as-is "into the centrifuge tube .

4. Rapidly add 80 ml. of distilled water, cap the tube and shake as quickly as possible to minimize lumps.

5. Let stand 10 minutes, inverting 3 times at 5 minutes and l0 minutes.,

6. Centrifuge for 15 minutes at 2000 rpm.

7. Separate the supernatant from the precipitated layer.

8. Weigh centrifuge tube containiaag precipitate layer.

9. Measure refractive index (RI) of supernatant and determine % d.s. using the RI-DS table for 1132 corn syrup (see CRA method E-54 available from the Corn Refiners Association, 1701 Pennsylvania Avenue, N.W., Suite 950, Washington, DC 20006).
The following calculations were made:
Weight of Sediment Hydration Capacity =
Weight of Sample (d.s.basis) Percent solubles = % d.s. of supernatant The products of the invention have a hydration capacity of at least about 5 and preferably at least about 7. The products of the invention also have a percent solubles of less than about 2, preferably less than about 1.5.
EXAMPLES
The work was completed using Wenger TX52 and TX80 extruders from Wenger Mfg., Sabetha, KS, U.S.A. Most of the work utilized the TX80 twin screw extruder having co-rotating screws, a 100 horsepower motor and a belt drive system. The extruder had a barrel jacket with multiple sections. The last three barrel sections were cooled using city water at 66-67°F. Starch was fed from a 300 lb.
stainless hopper though a preconditioning paddle screen into the extruder barrel. Ingredients were mixed in 200 lb. batches with a 1.5 horsepower DAY (trade-mark) ribbon blender and product was conveyed to the extruder with an AFC 2 horsepower inclined spiral feeder.

The screw elements were configured so as to use enough mixing elements at the discharge end to :keep pressure in the barrel as high as possible over a short distance. The configuration uses maximum motor torque, while minimizing thermal energy and heat build-up. Cooling water was manually adjusted to control temperature.
The screw element configurations included six mixing elements (three forward followed by three reverse) starting just behind a cone screw at the discharge end ~the extruder. Six forward flow mixing elements also were employed further from the discharge end, i.e. closer to the inlet. ~rll the remaia~ing elements were forward conveying screw elements.
Extrudate samples were ambient air dried and milled on a Fitz Model DS6 comminuting machine. Bests results were obtained when starch was milled using two passes. The first pass milling included a number three round hole screen (0.12" diameter). The second pass milling included a 0027 screen (0.02°7" diameter).
Moist extrudate samples collected the last day of the trial were dried in an air oven at 120'F for more than one day.
The degree of starch gelatinization present after.extrusion was measured using microscopy during and subsequent to extrusion trials to identify the effect of extrusion conditions on starch granules. Inspections of starch granules for birefringence gave a representation of the degree of gelatinization and number of raw starch granules. Particle size analysis was also used to characterize starch granules swollen beyond the normal 13-15 micron distribution.
1~

Example 1 Conventional unmodified corn starch was extruded alone and coextruded with sodium stearoyl lactylate, 10 D.E.
maltodextrin, sucrose, dextrins, waxy starch and gums.
These trials employed heat and shear, resulting in a highly soluble starch with limited dispersibility and swollen viscosity.
The trial used BUFFALO (trade-mark) 3401 unmodified corn starch from Corn Products, Argo, Illinois, U.S.A. and AMISOL
(trade-mark) 4000 waxy maize starch from Refinacoes de Milho, Sao Paulo, Brazil as primary ingredients. CASCO
(trade-mark) 7011 and 7071 dextrins from Casco Inc., Etobicoke, Ontario, Canada as well as Casco's 1910 (10 D.E.) maltodextrin were used as additives.
Locust bean and xanthan gum were obtained from Colony Import and Export Corporation, Garden City, NY, U.S.A.
Sodium stearoyl lactylate (ARDOTAN (trade-mark) SP55K) was purchased from Grinsted Products, Industrial Airport, KS, U.S.A. Pre-Hydrated gums were obtained from TIC (trade-mark) Gums, Belcamp, MD, U.S:A.
Trials were conducted on a WENGER TX52 twin screw corotating extruder. The barrel jacket was configured such that the last three sections were connected to a MOKON
(trade-mark) hot oil temperature controller. Starch was fed from a 300 lb stainless hopper through a preconditioning paddle screen to the extruder barrel. City water was metered into preconditioner for manual moisture control.
Ingredients were mixed in excess of 12 minutes in 100 lb batches with a 0.75 hp paddle mixer.
The experimental screw configuration is described in Table I which refers to the extruder elements illustrated in the ' CA 02417958 2003-02-20 drawings. The goal of the configuration was to use enough mixing elements at the discharge end to keep pressure in the barrel as high as possible over a short distance. This configuration uses maximum motor torque, while minimizing thermal energy and heat build up. Cooling was manually adjusted to control temperature.
Die configuration consisted of a single die with a five hole opening. Each hole was 5 in diameter.
Most extrudate samples were ambient air dried and manually crushed for transportation. Select extrudate samples 'sere later ground using a Mikro-Samplmill with a 0.027 screen.
Initial runs included extruding only unmodified SL1FFAL0 3401 corn starch. Subsequent runs included coextruding starch with sodium stearoyl lactylate, 10 D.E. maltodextrin, sucrose, dextrins, waxy starch, locust bean, xanthan, and prehydrated gums. waxy corn starch was also extruded as a primary ingredient with a similar protocol. Ingredients and conditions were chosen to provide a dispersible extrudate suitable for use in instantized hot beverages and other food applications.
Operating conditions and starting materials for the runs are shown in Table III. Starch feed rate for a majority of the runs was 34.3 kg/hr (8 revolutions per minute (rpm) feeder setting).
The minimum stable water addition rate was 3.3 kg/hr. Total moisture of the starch-water mixture entering the extruder barrel at these conditions ranged between 1~.3 and 20.2. Barrel rpm ranged between 160 and 212 depending upon operating conditions.
The Mokon hot oil unit maintained a Constant 120~C
temperature on the first two jacket sections (from the die plate) on the barrel. Temperature was held constant during the trial to obtain a fully gelatinized and expanded extrudate.
Die plate pressures typically ranged from 400 to 600 psig.
Percent extruder load (i.e. ~ electrical draw on the motor) ranged from 16 to 46depending on run conditions.
Preconditioner rpm typically ranged from Ft2 to 105 rpm.
The start-up procedure consisted of msing excess water with an initial starch rate. Starch rate was i.nc~eased to the desired setpoint with excess water. Finally, the water rate was reduced until the desired expansion of extrudate eras achieved.
Extrudate samples were inspected aftE;r the ingredients had been fed into the preconditioner for no leas thin 12 minutes.
Unground extrudate varied in color depending upon additive and composition. Most extrudate '°ropes°' mere brittle upon drying and cooling. Extrudate samples were only crushed for transporta-Lion. select samples were ground using ana Oo27 screen on a Mikro-Samplmill.
Example 2 The trial used Corn Products' BUFFAIuC~ 3401 unmodified Corn 2o starch. Locust bean and xanthan gum and Pre-Hydrated gums and other materials were obtained from the same sources as in Example 1.
The work was completed on a Wenger P.CX80 extruder. The Wenger TX80 twin screw extruder has corotating screws, 100 hp motor and a belt drive system. The extruder barrel jacket was configured with cooling and steam heat segments. City water (66°F) was varied manually for cooling on the last three barrel ' CA 02417958 2003-02-20 sections. Starch was fed from a 300 lb stainless hopper through a pre C and l t l on l ng padd l a s ~re a n ~ nt~ the extruder barre l s C~
ty water was metered into the preconditioner for moisture control.
Ingredients were mixed in 200 lb batches with a 1.5 hp Day ribbon blender. Product was conveyed to the extruder with an ~F'C 2 hp inclined spiral feeder.
The screw configuration is described in Table II which refers to the extruder elements illustrated in the drawings and, as with Example 1, it was designed to use enough mixing elements at the discharge end to keep pressure in the barrel as high as possible over a short distance.
Cooling water was manually adjusted to control temperature.
Die configuration consisted of one, single, round-hole, adjustable die with a 3y4 inch maximum diameter orifice. The diameter of the die orifice was adjusted to <0.344 inches (0.0929 sq. in.) and x0.281 inches (0.0620 sq. in.) opening.. Larger apenings would be required for increased production rates.
Extrudate samples were ambient air dried and milled on a Fitz Model DS6 Comminuting Machine. Best results were obtained when starch was milled using two passes. The first pass milling included a ~3 round hole screen (0.128 inch dia.). The second pass milling included a 0027 screen (0.027 inch dia.). Moist extrudate samples collected the last day of the trial were dried in an air oven at 120°F for more than a day.
The trial included extruding unmodified Corn Products~
HUFFALO 3401 corn starch. The starch was. also coextruded with locust bean, xanthan and Pre-Hydrated gum from. TIC gums.

' CA 02417958 2003-02-20 Ingredients and conditions were chosen to provide a dispersible extrudate suitable for instantized hot food applications.
Operating conditions and starting materials for the runs are shown in Table IV. Starch feed rate for a majority of the. trial was 4.6 lb/minute (17 rpm feeder setting). The minimum stable water addition rate during the trial was 0.408 lb/min. . Total moisture of the starch-water mixture entering the extruder barrel for these conditions ranged between 18.7 and 19.6%. The Wenger TX80 extruder barrel typically ran between 152 and 158 rpm.
The first two jacket sections (from the die plate) on the barrel were cooled manually with 57'F city water.
Die plate pressures typically ranged from 1200 to 1500 psig.
Percent extruder load ranged from f8 to 56% based on run conditions. The twin shaft preconditioner rotation was preset to 170 rpm.
The start-up procedure consisted of using excess water with an initial starch rate. Starch rate was increased to the desired setpoint with excess water. Finally, the water rate was reduced until the desired conditions were achieved. Extrudate samples 2~ were collected after a minimum of 12 minutes.
Extrudate "ropes" coming directly off the extruder were flexible~ Most extrudate samples were moderately brittle upon drying and cooling.
For best hot swollen viscosity results, extrudate samples were milled witty two passes on the Fitz I~S6 Comminuting Machine.
Two passes minimized any additional starch gelatinization due to heat build up in the mill. The first pass was.milled with a ,~3 2~

screen (0.128" dia.). The second pass was milled with an 0027 screen (0.027" dia.).
A control composition was prepared for purposes of comparative testing. The starting material starch was EUFFALO
3401 unmodified corn starch and at was processed in the Wenger TX80 twin screw extruder. Starch was fed at 4.6 lb/minute and water was added initially at about 1.I lb/minute and during processing was added at rates as low as about 0.2 lb/minute. The extruder was run at 34~40~ load capacity and an extruder rpm of 156-158. Temperature in the next to last section of the multiple section extruder was 176~F. ~ie plate temperature was f45-250'F
and die plate pressure was 1200 psig.
example 3 ANALYTICAL D APPLICATIQN TESTING
Light microscopy was used to provide visual confirmation of the degree of gelatinization being achieved. Samples were mounted in an immersion oil having a refractive index of 1.605 and viewed at 100X, 98~ crossed polars. The extrudates also were tested for both hot and cold applications.
During the first day of operation, small batches of material reflecting a variety of extrusion conditions were prepared.
Extrusion conditions for all runs are listed in Table Ice.
Photomicrographs of these materials vs. the control composition were evaluated and it was observed that the control extrudate produced contained material ranging from uncooked, raw starch granules through partially gelatinized to fully cooked pieces.
Partially polarized images showed raw starch (Maltese crosses), through partially gelatinised (some birefringence) to totally cooked particles (no birefringence) in a heterogeneous mixture.
Material 312-lA (Table IV) was extruded at the lowest temperature of all the prototypes processed the first day, 159'F.
A photomicrograph of the material exhibited some individual raw starch particles with the majority of material being partially to fully cooked starch.
Extrudate 312-1M (Table IV) (single-pass milling) was processed at higher temperature (259-F), lower pressure, and photomicrographs showed large site pieces tending toward a more cooked appearance with many more individual raw starch granules with Maltese crosses. Particles displaying an intermediary degree of cook were not as evident as they were in the 312-lA
sample. 312-1H (Table IV) (double-pass milling) showed a greater amount of individual, uncooked, raw starch granules than in the single-pass material..
Extrudate 312-J (Table IV) was processed at the highest temperature evaluated, 266'F. For the majority of fields viewed, small pieces of individual, raw starch were the prevalent birefringent particles. Typically, large pieces were completely cooked.
For the hot applications, 30,g of agglomerated material (extruded starch, maltodextrin, sugar) were mixed unto 200 ml hot liquid with continuous stirring: Ease o1: dispersion and the rate and degree of viscosity formed were observed. Mouthfeel, body, and cooked flavor of the formulation were also noted. For comparison purposes, both a positive control using the control ' CA 02417958 2003-02-20 seemed to thicken more immediately and provide more body. 312-1H (Table IV), both single and double-pass milled, was not as thick as the 312-lA, 1B (Table IV).
In the cold formulations, just the opposite seemed to be the 20 case. In cold water formulations, starches extruded at the higher temperature seemed to thicken more. 312-1H (Table IV) (single and double-pass milled) seemed to thicken more than 312-lA and 312-1B (Table IV). All of the cold formulations were kept in the refrigerator overnight at 38~F. Although the suspension 25 was maintained, some water did migrate to the surface. Sample 312-lA (Table IV) exhibited the highest water level: Samples 312-th (single and double pass) and 312-J (Table I'V.), the Lowest. In ' CA 02417958 2003-02-20 all cases, the emulsion could be easily reformed by simple hand stirring. The trials indicate that extrusion at higher temperatures enhances starch solubility in cold liquids.
Haake viscosity and particle size analyses were also utilized to compare certain samples With the control composition.
These analyses were conducted on samples formulated for cold application testing. ~Isake viscosity at 25~~ was run 15 minutes after sample addition to the cold water. results for the application tests COnduCted on the 313~2~, 313°2C, and 313-2H
(all Table IV) samples are summarized as follows:
Although viscosity data for the test batches did not meet the value obtained for the control composition, they were substantially better than the products of Example 1.
Particle size distribution patterns were visually compared.
Sample 313°2A (Table IV) seemed to have a distribution most similar to the control composition and in hot application tests performed most like the control. As noted with the prototype evaluation a day previous, the starch extruded at higher 2'~

temperatures (313-2H, Table IV) hydrated more quickly and provide more viscosity in the cold formulations.
The extrusion trials demonstrated tb.e ability of the extruders to process moderate moisture starch under relatively high pressure to produce a cold or hot water swellable product.
Example 4 MICROSCOPY
Two samples of the product of the invention, 313-2C
and 314-3S (both Table IV) were examined by microscopy and comparative examinations were made of commercial pre-gelatinized corn starch and commercial, spray-dried, modified corn starch.
Two media were used for mounting the samples.
CARGILLE (trade-mark) liquid 1.604 (available from Cargille Laboratories, 55 Commerce Road, Cedar. Grove, NJ 07009 U.S.A.) is an oil with a refractive index of 1.604. The oil keeps the samples from dissolving or swelling. The refractive index, much higher than that of the particles, increases the contrast for viewing and photography. The other mountant was 1:1 glycerin to water. The water swells the particles, and the glycerin prevents evaporation. The swollen starch particles have a refractive index close to that of the mountant (glycerin and water) so the contrast was very low.
Sample 313-2C
Mounted in oil, the particles are colorless, transparent to translucent, irregular chips. kith partially crossed polarizing filters, it can be seen in Fig. 16 that some of the particles are recognized by shape, harsher edge contrast, more "solid"
appearance as seen in Fig. 17 and, with the polarizing filters crossed, by their residual birefringence as seen in Fig. 18. The completely gelled starch particles swell into soft, pulpy slabs 15 with no birefringence and only a little texture. Faint graininess typical of gelled starch is seen and, in some swollen particles, faint, irregular striations. ~f particular interest are the intermediate, partially gelled, partially swollen particles, those that have lost most of their birefringence but 2~ retained a lumpy texture. In these particles or portions of particles, clusters of swollen granules can be seen. The contrast is stronger in these areas. These areas of partial swelling vary from being quite distinct (swollen and even raw granules visible) to being crowded.and pushed together so that no 25 individual granules can be distinguished. It is thought that this component of the sample is imp~rtawt to the thickening properties, as it has the ability to absorb water and swell yet retain some substance and strength.
Sample 314-3S
This sample ~is similar to Sample 313-2C in that it contains l the same inhomogeneous variety of particles, ranging from completely gelled starch td raw granules. however, this sample appears to contain a high amount of the intermediate, partially gelled particles. Mounted in oil, there are few free raw granules as seen in Fig. 19. There are also a few completely isotropic chips with absolutely no birefringence (brightness).
However, many particles are aggregates of granules.
Mounted in water and glycerin, this sample has the same types Of particles aS Sample 3I3-2C, but the r8ti0 of the types is different. There is-more of the partially swollen, lumpy material. Fig. 20 is a photomicrograph of the sample in glycerin and water and Fig. 21 is a photomicrograph of the sample in glycerin and water taken with the polarizing filters.
Commercial Pre-gelatinized Corn Starch This product was examined for comparison. Mounted in oil, it is seen to contain similar chip morphology to the product of the invention (although it has been ground to a smaller average particle size). With partially crossed polar~izers, however, it is seen to contain no birefringent particles, neither individual granules nor aggregates as seen in Fig. 22. The particles are uniformly isotropic. This product is quite uniform in degree of starch gelling, i.e. it is completely gelled.

~

Mounted in water and glycerin, the particles uniformly swell into soft slabs with only a faint, fine, grainy texture. No hint of granules remains. Fig. 23 is a photomicrograph of the sample in glycerin and water and F°ig. 24 is a photomicrograph of the sample in glycerin and water taken with the polarizing filters.
Commercial, Spray-dried, Modified Corn Starch This product also was examined.for comparison. Mounted in oil, the particles are seen to be completely isotropic as seen in Fig. 25. The particles show the entrapped air bubbles typical l0 for spray dried materials. Spray drying also results in rounded particles. This effect can be seen to some degree in these particles. They are not simple spheres, but they do have generally rounded shapes.
Mounted in water and glycerin, this product swells uniformly. No birefringence remains, but chemical modification restricts the swelling so that the granules retain some integrity. The swollen particles have a lumpy texture similar to the product of the invention, but produced by chemical treatment.
Fig. 26 is a photomicrograph of the sample in glycerin and water 2~ and Fig. 27 is a photomicrograph of the sample in glycerin and water taken with the polarizing filters.
example 5 AGGLOMERATION
An agglomeration method was.developed to prepare a composition useful in instantized applications and the method can be used with the physically modified products of the invention and with other starch containing materials such as fully pre-31.

gelatinized starches. The method requires a specific ingredient addition sequence. ~ core component such as a crystalline highly soluble material, a sugar or a derivative of sugar is placed in a mixer and water is added in an amount from about 0.5% to about 3.5% by weight of the total weight of the ingredients, excluding the weight of the added water. The core component and added water then are blended by mixing. The amount of core component employed is from about 7% to about 69%, based on total ingredient weight excluding added water, and depending on the ax~ounts of to other ingredients the core material can be present in an amount from about 9 to about 69%, preferably from about 7 to about 52%.
Suitable core components are selected~from the group consisting of dextrose,_sucrose, fructose, maltose, lactose, galactose and other mono- and di-saccharides. Sugar alcohols also can be used.
The next component which is added to the mixer is a non-crystalline soluble material. Suitable materials of this type are selected from the group consisting of maltodextrins, corn syrup solids, polydextrose and soluble dextrins. The non~
crystalline soluble material is added in an amount from about 1%
to about 20%, preferably from about 3% to about 10%, based on total ingredient weight excluding added water. This component and the others then are blended by mixing.
The last component which is added to the mixer is a starch containing material such as the physically modified product of the invention or a fully pre-gelatinized starch or the like.
This component is added in an amount from about 90% to about 30%~
preferably from about 90% to about 45%, based on the total ' CA 02417958 2003-02-20 ingredient weight excluding added water. This component and the others then are blended by mixing to male the agglomerated product of the invention.
The experimental work utilized a bench-top Hobart mixer. A
crystalline, highly soluble material (such as sugar) is wetted sufficiently to provide: a core onto which an intermediary ingredient, soluble but: not crystalline (such as maltodextrin) is then blended. Finally, the primary component (the product of the invention) is added to the system. The order of addition and degree of blending are critical to produce a granular type product that is homogeneous, flowable and easy to disperse in hot media: The concentration of ingredients is adjusted to yield the highest starch load. Carrier ingredients are selected for their morphology, ease of solubility and appre~priateness in the application being formulated.
The formula tested consisted of 33% sugar, 60% of the product of the invention and 7% maltodextrin. The sequence of steps was as followsm 1 Place sucrar in Hobart mixer.
2. Sprinkle water on the sugar in an amount equal to 2.5% of the total dry ingredients, i.e., for a blend of 50 grams of sugar, 9C~ grams of extruded starch and 10 grams of maltodextrin the water would equal 3.75 grams (2-1/2% of 150 grams).
3. Mix on speed 2 until completely blended.
4. Add maltodext:rin while mixing at low speed.
5. Mix on speed 2 until completely blended.

~' CA 02417958 2003-02-20 6. Add extruded starch while mixing at low speed.
7. Mix on speed 2 until completely blended.
This agglomeration procedure in combination with the formulation noted above results in a premix having the following characteristics:
1. A good granular appearance and stability of the blended ingredient.
2. A homogeneous mixture which does not stratify.
3. Premix is flowable and easy to measure.

T~LFr I
WENG ER 8 ~ SCRL~1 TK CON
~~URIiTION

1 Flg. 4 CONE SCREW

2 F 1 11 THI CK SHE~IRI,OCK
g .

3 Fig. 12 THICK SHEARLOCK

4 ~ Fig 13 THICK SHEARI:OCK
.

5 Fig. 12 THICK SHEhRLOCK

. 6 Fig. 11 THICK SHEA,RLOCK

7 Fig. 12 THICK SHEhRLOCK

8 Fig. 5 FULL PITCH SCREW

Fig. 5 FULL PITCH SCREW

10 Flg. 5 FULL PITCH SCREW

11 Fig. 5 FULL PITCH SCREW

12 Fig. 5 FULL PITCH SCREW

13 Fig. 5 FULL PITCH SCREW

14 Fig. 5 FULL PITCH SCREW

15 Fig. 6 FULL PITCH SCREW

16 Fig. 12 THICK SHEARLOCK

17 Fig. 11 THICK SHFARLOCK

18 Fig. 12 THICK SHEARLOCK

19 . Fig. 13 THICK SHEARL4CK

20 Fig. 12 THICK SHEARLOCK

21 Fig. 11 THICK SHEARLOCK .

22 Fig. 5 FULL PITCH SCREW

23 Fig. 5 FTJLL PITCH SCREW

24 Fig. 5 -FULL PITCH SCREW

25 Fig. 5 FULL PITCH SCREW

DRIVE

END a I 1 TL~ II
WE NGER X 52 S EILEliENT CONFIGURATION
T

1 Fig. 9 TRIPLE FLIGHT
CONE SCREW

2 Fig. 8 1/2 PITCH SCREW 6 UNITS

3 Fag. 15 THIN SHEARLOCK

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to s Fig. 14 THIN sHEARLOCx Fig. 15 THIN SHEARLOCK

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16 Flg. 15 THIN SHEa~RLC)CK

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18 Fgg. 15. THIN SHEARLOCK

19 Fig. 14 THII~1 SHEARLOCK

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23 Flg. 14 'THIN SHEARLOCK

24 Flg. 15 THIN SHEARLOCK

25 Flg. 14 THIN SHEARLOCK

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27 Flg. 7 1/2 PITCH SCREW 9 UNIT

28 Flg. 3 3/4 PITCH SCREW 9 UNIT

2~ Flg. 3 3/4 PITCH SCREW 9 UNIT

30 Flg. 3 3/4 PITCH SCREW 9 UNIT.

31 Flg. 10 3f4 FITCH SCREW 4.5 UNIT

DRI~IE

END

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Claims (9)

CLAIMS:

1. An agglomerated composition which is homogeneous, flowable, and easily dispersible in hot instantized applications comprising - a starch containing material;

- a core component; and - a soluble non-crystalline material.

2. The agglomerated composition of claim 1 wherein the starch containing material is - a physically modified starch composition comprising a heterogeneous mixture of starch particles which are fully gelatinized, partially gelatinized and raw, and having a hydration capacity greater than about 5 and percent solubles less than about 2.

3. The composition of claim 2 wherein the core component is selected from the group consisting of dextrose, sucrose, fructose, maltose, lactose, galactose, mono- and di-saccharides and sugar alcohols and the soluble non-crystalline material is selected from the group consisting of maltodextrins, corn syrup solids, polydextrose and soluble dextrins.

4. The composition of claim 2 wherein the physically modified starch composition is present in an amount from about 90% to about 30%, the core component is present in an amount from about 9% to about 69% and the soluble non-crystalline material is present in an amount from about 1% to about 20%.

5. The composition of claim 2 wherein the physically modified starch composition is present in an amount from about 90% to about 45%, the core component is present in an amount from about 7& to about 52% and the soluble non-crystalline material is present in an amount from about 3% to about 10%.

6. A method of making an agglomerated composition which is homogeneous, flowable and easily dispersible in hot instantized applications, employing as ingredients a core component, a soluble non-crystalline material and a starch containing material, comprising the sequential steps of - adding a core component to a mixer;

- adding water in an amount from about 0.5% to about 3.5% by weight of the total weight of the ingredients;

- mixing until completely blended;

- adding a soluble non-crystalline material while continuing mixing until completely blended;

adding a starch containing material while continuing mixing until completely blended.

7. The method of claim 6 wherein the starch containing material is a physically modified starch composition comprising a heterogeneous mixture of starch particles which are fully gelatinized, partially gelatinized and raw, and having a hydration capacity greater than about 5 and percent solubles less than about 2.

8. The method of claim 6 wherein the core component is selected from the group consisting of dextrose, sucrose, fructose, maltose, lactose, galactose, mono- and di-saccharides and sugar alcohols and the soluble non-crystalline material is selected from the group consisting of maltodextrins, corn syrup solids, polydextrose and soluble dextrins.

9. The method of claim 7 wherein, excluding adding water, the physically modified starch composition is present in an amount from about 90% to about 30%, the core component material is present in an amount from about 9% to about 69%
and the soluble but not crystalline material is present in an amount from about 1% to about 20%.