NZ197228A

NZ197228A - Free-flowing anhydrous dextrose and production from starch hydrolysate

Info

Publication number: NZ197228A
Application number: NZ197228A
Authority: NZ
Inventors: L R Idaszak; K J Bernatz
Original assignee: Cpc International Inc
Priority date: 1980-06-03
Filing date: 1981-05-28
Publication date: 1984-07-31
Also published as: NL8102644A; JPH0333320B2; KR850001355B1; JPS5722699A; IN155230B; NL189921B; YU140081A; SE455506B; FR2483427A1; YU41244B; DE3121918A1; ES8203968A1; FR2483427B1; GB2077270B; ZA813716B; AR227782A1; AU548023B2; SE8103441L; AU7128781A; IT8121991A0

Description

<div class="application article clearfix" id="description"> New Zealand Paient Spedficaiion for Paient Number 1 97228 % I Priority DEte{s): <3•; . PP. Completo Spsciiication Filed: Class: . Pi '.r'.K/'.Q Publication Dato: . 5A.JPL1984... P.O. Journal No: .. NEW ZEALAND PATENTS ACT, 1953 No.: Date: COMPLETE SPECIFICATION "FREE FLOWING CRYSTALLINE HIGH DEXTROSE BEARING PRODUCT" kl We, CPC INTERNATIONAL INC., a corporation organised under the laws of the State of Delaware, U.S.A., located at International Plaza, Englewood Cliffs, New Jersey 07632, U.S.A. hereby declare the invention for which S / we pray that a patent may be granted to pik/us, and the method by which it is to be performed, to be particularly described in and by the following statement:- - 1 - (followed by page la) FREE FLOWING CRYSTALLINE HIGH DEXTROSE BEARING PRODUCT BACKGROUND OF THE INVENTION Field of the Invention The present invention relates to a free flowing, handleable, crystalline, anhydrous high dextrose bearing product, and particularly relates to a solid high dextrose bearing product which has composition stability and does not cake after prolonged storage. The Prior Art Solid dextrose is conventionally manufactured by crystallizing super-saturated, high dextrose syrups and recovering the crystals therefrom in alpha-dextrose mono-hydrate crystal form. This process is described in U. S. Patent No. 3,039,935. Yields depend on carefully controlled cooling temperatures and dextrose super-saturation conditions. Complete recovery of the dextrose from the syrup cannot be accomplished by this process because effective dextrose crystallisation and separation therefrom requires supersaturated dextrose solutions. Accordingly, as dextrose is crystallized out of the solution it becomes dilute and a significant portion of the dextrose therefore remains in the syrup (the mother liquor) upon completion of the dextrose crystallization step. Anhydrous alpha-dextrose is generally manufactured from the crystallized dextrose by dissolving the alpha-D-dextrose monohydrate crystals therefrom in water and -1« crystallizing at temperatures of 60-65°C in vacuum pans under carefully controlled processing conditions. It is known to manufacture such anhydrous alpha-dextrose from hydrolysates containing greater than 96% dextrose, dry substance(hereinafter "d.s.")basi A process for solidification of all the solids in a conversion syrup without separating the dextrose therefrom has been described in U. S. Patent No. 3,197,338 which discloses a process for producing a crystalline, non-caking dextrose product. In the '338 patent, a refined dextrose conversion syrup is concentrated to at least 95% d. s. (preferably greater than 98% d. s. ) crystallized by kneading at 170-230°F and extruded in the form of ribbon or strand into a zone which rapidly cools the product to less than 150°F. The extrudate is then granulated to an appropriate particle size. In U. S. Patent No. 3,236,687, dextrose conversion syrup solids are reportedly converted into a solid form by subjecting a syrup concentrate at a 93-96% d. s. level and 180-220°F to high shear in the presence of gas to form minute glucose crystals. The result is described as a nucleated, creamy, frothy dextrose mass. This mass is deposited on a moving belt and solidified in a series of cooling zones which are maintained at progressively lower temperatures (e.g., first zone at 180-220°F, second zone at 14Q-180°F, and third zone at less than 100°F.) The solidified mass is chipped, conditioned for two to three hours at 120-180°F, ground and redried. Another prior art method of producing granular dextrose involves a three step process wherein a liquid hy-drolyzate is contacted with seed material in a mingler or mixer followed by casting the material onto a continuous belt where it is cooled and transformed into a solid sheet. The sheet is then crushed and sometimes given an additional cure on another continuous belt. This process is described in U.S.Patent No. 3,650,829. U.S. Patent No. 4,059,460 describes another process for preparing a solid anhydrous dextrose. This process comprises preparing a molten dextrose syrup concentrate having a d.s. concentration from 85% to 93% and a temperature in excess of 230° F. The concentrate is shear mixed and cooled to a temperature below 200°F. to form a more viscous but fluid dextrose mass. This fluid dextrose mass is maintained at a concentration below 93% d.s. and a temperature above the dextrose hydrate crystallization temperature. It is then shaped, ribboned or deposited on a belt, and transformed into a solid mass. The solid mass is then granulated and dehydrated to a water content of less than 2%. Anhydrous dextrose products prepared directly from hydrolyzates and containing the non-dextrose higher sugars in accordance with the prior art have been generally unsatisfactory due to caking and handling problems. They are difficult to ship in .bags due to their caking tendencies. Moreover, they cannot be bulk shipped in hopper cars due to poor flow characteristics which make unloading difficult or impossible. According to the present invention, the steps of mixing liquid hydrolyzate with optional seed, transformation to a solid and crushing are carried out in a single, continuous, heavy duty mixer and are therefore effectively combined in one step. The product from this step is then conditioned to impart handle-ability and composition stability. SUMMARY OF THE INVENTION A free flowing, handleable, crystalline, anhydrous high dextrose bearing product is prepared continuously from a concentrated starch hydrolyzate. According to the process, the concentrated starch hydrolyzate is added to a heavy duty mixing device (seed material can be added as an option at this point in the process) wherein it is transformed - 3 - 1Q^OOo i fC 4 b to a crystalline form, crushed and cooled in a first step. The crushed crystallized product is then further cooled and milled and can be screened if necessary. Finally, the crushed, milled and optionally screened crystallized product is conditioned by drying to reduct total moisture content. The tern "high" as used herein in relation to dextrose bearing products means those products being at least 85% dextrose by weight. DETAILED DESCRIPTION OF THE INVENTION The starch hydrolyzate utilized in the present invention can be prepared by conventional means such as by enzymatic or acidic hydrolysis of starch. Concentration of the hydrolyzate to a d. s. concentration of from about 92% to about 99% preferably from about 95% to about 99%, is then carried out by, for example, evaporation in a wiped film evaporator. This concentrate will be referred to in the present specification as "concentrated starch hydrolyzate". Concentrated starch hydrolyzate at a temperature from about 90 °C. to about 135°C, is added to a heavy duty mixing device with a jacket to remove both sensible heat for cooling and the exothermic heat of crystallization. About 1% to about 15% of a seed material td,s,basis) caa ibe added simultaneously if necessary, or desired. Mixing is carred out for from about 1 minute to about 1 hour. Seed material can be any crystalline sugar or previously prepared free flowing, handleable anhydrous high dextrose bearing product. The continous process becomes self seeding after a short period of operation and therefore seeding is generally unnecessary. Several heavy duty mixing devices that are suitable for the present invention are commercially available. These include the Readco Continuous Processor manufactured and sold by Teledyne Readco. The devices are provided with jackets for heat removal. Jacket temperature is maintained at from about 2 0° C. to about 409 C. according to the present invention. Additional heat removal capacity can be provided by means of a heat exchanger connected in series with the heavy duty mixing device. Any conventional scraped surface heat exchanger, such as the VOTATORV scraped surface heat exchanger manufactured and sold by Chemetron Corpora- f tion, is suitable. Mixing of the concentrated starch hydrolyzate and optional seed material produces a crushed crystalline product that is dry and granular and is characterized by a particle size ranging from powder to about 2 inches in diameter. Sufficient cooling is carried out during mixing to provide crushed product at a temperature from about 80° C. to about 110° C. The crushed crystalline product is then preferably cooled to below about 30° C, This can be done in, for example, a jacketed blender sparged with cooled, conditioned (.i.e. low humidity) air. The cooled crystalline product is then milled to a reduced particle size by conventional means. Screening is necessary only if a specific particle size is required. The crushed, milled and optionally screened crystalline product is then conditioned in two stages. A fluid-ized bed is used in the first stage wherein the crystallized product is fluidized for a residence time from about 7 to about - 5 - 197228 45 minutes preferably fro. atout 7.to about 15 minutes at a teopsrature from about 65° to about 120 c- to obtain a product with less than about 0.5% total moisture. The second conditioning stage includes cooling the product from the elevated temperature of the first conditioning stage to below about 35° C. This is done in the present invention by either a second fluid bed treatment or during pneumatic transport, both preferably with dehumidified air. Other equipment for conditioning which accomplishes the same moisture reduction can be used. The final conditioned high dextrose bearing product has excellent handleability and composition stability. Several characteristics of the product of this invention can be measured. These include dextrose content, moisture content, alpha- and beta-anhydrous dextrose.content, crystallinity, particle size and handling characterisitics. Typical values for these measurements are disclosed in this specification in the examples. Dextrose content can be measured by conventional HPLC (high performance liquid chromatography). Moisture and particle size are also measured by conventional means. The product is anhydrous because of the elevated temperature used in transformation. More than about 50% of the product is in the beta-anhydrous form with the remainder in the alpha-anhydrous form due to the low moisture, high rate tansformation. The alpha-and beta-anhydrous dextrose fractions are determined by NMR (nuclear magnetic resonance). Crystallinity is a measure of the crystalline, or non-amorphous, structure of the product. Crystallinity is determined from heat of fusion -measurements using a DSC (differential scanning Calorimeter). Samples of alpha-anhydrous dextrose prepared by conventional crystallization were used as standards for completely crystalline material. Product crystallinity was determined by comparing the heat of fusion of the product with that of a crystalline standard having the same percentage of alpha- and beta- dextrose as that of the sample. This corrects for the difference in heat ' 20 JUKf953 6 of fusion between alpha- and beta-anhydrous dextrose. The product handleability is characterized by use of the Jenike Test Method, a laboratory method which quantifies the flow and storage properties of bulk solids. (See "Know Your Material - How to Predict and Use the Properties of Bulk Solids", Chemical Engineering/Deskbook Issue, J. R. Johanson, October 30, 1978 and "Flow properties of Bulk Solids", ASTM, Proc., Vol. 60, 1960, pp. 1168-1181.) "Test results for the product are compared with results for alpha-hydrate dextrose made by conventional crystallization. Experiments were conducted with a DSC and SEM (scanning electron microscope) to compare subjectively the handleability of the product of the present invention and a typical product from a belt transformation process which exhibited excessive caking tendencies. The product of the present invention had a higher, better defined crystal structure and a better dispersion of the amorphous phase compared to the belt product. Both of these factors are considered to contribute to the excellent handling properties of the product of the present invention. The following examples are provided to further describe the invention. EXAMPLE I Starch hydrolyzate was concentrated to at least 90% d.s. with a wiped film evaporator (except in Test No. 1 in Table I which utilized a syrup prepared by dissolving crystalline anhydrous dextrose followed by concentration to 85.3% d.s. in a wiped film evaporator). Concentrated starch hydrolyzate was then transformed into a solid in several batch tests using a double arm, overlapping, Sigma blade, jacketed blender manufactured by Teledyne - 7 - Readco. The blender consisted of a rectangular trough with a curved bottom that formed two longitudinal half cylinders and a saddle. It was equipped with two Sigma type blades which revolved toward each other with overlapping circles of rotation. The blender had a six quart working capacity and a nine quart total capacity. Conditions and results are tabulated in TABLE I. Anhydrous dextrose was used as seed for tests No. 3, 4, 5 and 6. No seed was used in test No. 1. The product from test No. 1 was used as seed for test No. 2. The batch blender was overfilled in tests number 1 and 2 which prevented the agitators from effectively kneading and shearing all of the material. Higher jacket temperatures in those tests also contributed to longer transformation times. When the charge was reduced to about 4 kg. and the jacket temperature to about 6 0°C, transformation time was reduced significantly. The crystalline dextrose products had caking tendencies. EXAMPLE II A continuous process was demonstrated in a Readco Continuous Processor manufactured by the Teledyne Readco Company. The mixing chamber was 3 6 inches long and consisted of twin cylindrical chambers 5 inches in diameter. Two parallel shafts of agitators that rotated in the same direction were employed by the processor. The blades on one agitator were lens shaped and maintained close clearances with the second agitator, 90° out of phase with the first, as well as with the walls of the chamber. This not only assured a sufficient mix but also provided a self-cleaning action of the agitator blades. A full jacket was provided on the chamber for cooling of the material being-blended. Hydrolyzate feed time for each continuous run averaged about five minutes. The results of some early tests are summarized in TABLE II. Supply Charge a) to Test Concentration, Dextrose, Blender, No. % d.s. % d.b. kg 1 85.3 100.0 6.69 2 '95.2 93.8 5.78 3 97.7 94.0 3.06 4 98.1 96.1 4.65 1 5 96.2 98.1 3.63 lo 6 97.2 98.1 4.08 i a) % d. b. means % d. s. basis TABLE I Product Transfor- Blender Beta mation Jacket Crystal- Anhydrous Seed, Time, Temp, Moisture, Unity, Dextrose % min. °C % $ as-is % d . h. 0 150 100 0.1 100.0 25.4 10 97 100 0.2 30 75.8 10 12 60 1.1 76 57.2 10 13 60 0.7 81 59.3 10 5 60 3.2 79 51.1 10 12 60 1.4 80 57.9 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 TABLE II Blender Rate, Residence Jacket Crystal- Concentration, Dextrose, kg/ Seed, Time, Temp. Moisture, linity, % d.s. % d.b. min. %d.b, min. "C % % d.b, 95.9 90.7 1.44 10 - 60 1.8 67 89.5 99 .4 1.33 9.8 1.0 40 0.6 88 92.3' 99.2 1.45 9.3 2.2 40 0.4 94 94.7 98.9 1.16 11.5 3.9 40 0.2 96 96.4 - 0 . 94 14 1.9 38 0.9 89 96.3 - 1.45 9 1 38 0.8 86 95.4 - 0.88 15 2.5 38 0.7 92 96.3 - 1.43 9 1.5 38 0.9 93 96.2 - 1.40 9 0.75 38 0.9 92 96.2 94.5 1.20 11 8.5 38 1.9 77 96.8 94 . 4 1.33 10.2 1 24 1.3 81 96.8 94 .3 1.18 11 4.5 32 2.8 76 94.7 92.7 1.48 9 1.6 27 2.6 77 94.1 92 . 4 1.42 9.5 1.5 18 1.7 78 96.9 94 . 8 1.23 11 5 24 1.8 78 96.6 94 . 8 1.30 10 8 24 1.5 81 95.4 98 . 5 1.33 10 2.7 2.7 3.2 91 95.8 98.7 1.35 10 1.5 24 2 . 2 93 96.0 98.6 1.40 9.7 1 24 ■ 1.9 84 95.9 98.0 1.35 10 1.5 24 2.2 92 The supply for tests number 5 through 9 was dissolved anhydrous dextrose. Seed material for all of the tests was crystalline anhydrous dextrose. The crystalline dextrose product had caking tendencies. EXAMPLE III A sample was prepared incorporating all process steps of the present invention. A 5 inch diameter Readco Continuous Processor was used followed by subsequent milling and conditioning in a single tube three inch diameter five foot high fluid bed. Product analysis and nonscreened particle size analysis were as follows: PRODUCT ANALYSES d.s.,%: 99.6 dextrose, %d. b. 98.2 Beta-anhydrous dextrose, % d.b.: 51.1 crystallinity, % as-is: 92 color (40° Be): 1.1 ash (SO4), % d. b.; 0.01 SCREEN ANALYSIS % Retained on U. S. Sieve Mesh Size 20 40 60 100 140 200 pan 6.8 25.4 22.0 14.6 12.4 1.8 16.0 The Readco Processor was operated for a little over one hour at a production rate of about 5 lbs. per minute without using seed. The product from the Readco Processor consisted of hot, agglomerated material up to about 2-inches in size. This material was spread out and allowed to cool to ambient temperature over a period of about 1 hour and then milled on a single pass with a Fitz mill. The milled product was first -11- conditioned in the fluid bed with a residence time of about 15 minutes at 65°C. to reduce the total moisture to less than about 0.5%. This treatment was followed by a second pass through the fluid bed under conditions to cool the final product below 35°C. A portion of the sample was used to fill a 100 pound, three-ply, polyethylene lined bag. The bag was then placed under five 100 pound bags of anhydrous dextrose to simulate the weight of a pallet shipment. After 37 days, the bag was opened and the sample material had what may be described as a "soft set". That is, lumps could easily be broken by hand. EXAMPLE IV ■ A series of samples were prepared according to the complete process described in Example III at different levels of dextrose content. Product analyses were as follows: Test Dex., Moist., B-anhydrous Crystallinity Ash. No. %d. b. % dextrose,% d. b. % as - is % d.b. 1 98.7 0.2 67 .5 93 0.01 2 98.1 0.3 61.3 89 0.02 3 94.6 0.8 66.7 62 0.37 4 93.8 0.5 70.2 73 0.02 A 10 0 lb. sample of each was placed in a bag as in Example III. The bags were then each stored under twenty 100 lb. bags of dextrose in a plant warehouse. After more than two months, the bags were inspected and found to have developed no more than a soft set. The product from test 3, which was at 0.3% moisture -12- (inadvertently above the desired less than about 0.5% moisture) was slightly caked compared to the other three. EXAMPLE V A series of conditioning tests were conducted to impart handleability (non-caking characteristics) to products made according to the. process described in the foregoing examples. Conditioning was carried out in a three inch fluid bed. Process temperatures were achieved with either hot water or steam in a jacket on the fluid bed. Fluidizing air was introduced through a bottom distribution plate with 28 holes 1/16-inch in diameter at a superficial fluidizing velocity of 2 ft. per second (70°F, 1 atmosphere). The results appear in TABLE III. EXAMPLE VI Two samples were prepared according to the complete process described in Example III. The supply hydrolyzate contained 95.9% D.B. dextrose, the product from the Readco Processor for the first smaple had a 98.9% D.S., 74% as-is crystallinity and 57.7% D.B. 3-anhydrous dextrose, and for the second sample had a 98.9% D.S., 73% as-is crystallinity and 61.9% D.B. B-anhy-drous dextrose. The first sample was conditioned in fluid bed at 99°C for 18.6 minutes. This gave a conditioned product having a 99.6% D.S., 77% as-is crystallinity and 58.5 D.B. 3-anhydrous dextrose. The second sample was conditioned in the fluid bed at 118°C for 7.7 minutes. This gave a conditioned product having a 99.6% D.S., 74% as-is crystallinity and 63.3% D.B. 3-anhydrous dextrose. -13- I TABLE III SUPPLY ANALYSES a) PROCESS CONDITIONS PRODUCT ANALYfiVS Test d.s., % Beta anhyd. dex. % d.b. Cryst., % as is Temp. °<C Time, min. d.s. % , Deta anhyd. dex., % d.b . cryst. % as is 1 98.9 54.2 89 107 15 99.6 53.9 87 2 98.9 54.2 89 107 45 99.9 54.0 87 3 98.1 49.8 86 87 30 99.3 50. 6 93 4 98.1 49.8 96 66 15 99.4 51.3 90 5 98.2 54.5 81 6€ 45 99.6 55.2 86 6 98.2 54.5 81 87 30 99.8 55.7 87 a) The supply material was prepared in accordance with the process described in Example III. The material was processed with as-is particle size from milling without screening. The results of conditioning are limited primarily to a reduction of total moisture. No appreciable changes in final product composition (beta-anhydrous dextrose and crystallinity) were apparent. EXAI4PLE VI I Tests were conducted to determine the effects of moisture, storage temperature and storage time on the crystallized dextrose products. Crystallinity contents of both conditioned and.non-conditioned products were also evaluated. Three test batches were prepared. Each batch involved operation of a Readco Continuous Processor to give a product at a different moisture level (3.6%, 1.9% and 0.9%). The product from each series was separated into two parts and handled as follows: 1. One part was stored as is at ambient temperature. 2. The second part was fluid bed conditioned on the day it was made. All products were analyzed when made and then again at the invervals shown in the table. The results are summarized in TABLE IV. -15- TABLE IV Batch No. Sample . Description Analyses Age, Davs ' Moisture % Beta Anhydrous Dextrose % d-b« Cryst. % as-is 1 Product (1 If 0 13 31 3.6 53.7 12.0 7.2 85 Conditioned Product II II fl II 0 13 31 0.4 0.4 0.3 50.3 47.6 49.8 92 2 Product II II 0 14 32 1.9 1.7 1.5 61.8 9.8 8.9 87 Conditioned Product fl II II II 0 13 31 0.3 0.3 0.3 61.0 58.5 60.4 86 ' 3 Product II Tf 0 14 27 0.9 1.2 0.8 62.6 21.1 24.5 32 Conditioned Product if If II II 0 14 27 0.3 0.4 0.4 61.2 64.6 65.2 84 a) All samples were prepared at the same Readco Continuous Processor throughput rate of about 5 pounds per minute without seed. Product temperatures for batches 1, 2 and 3 were 91°C., 93°C. and 99°C. , respectively, b) Days analyses conducted after sample originally made. c) High moisture is an abberation. The following conclusions were drawn from the foregoing results. 1. There were no appreciable differences in initial product beta-anhydrous dextrose content with moisture level. The small -16- differences are probably attributed to mutarotation before analysis of the higher moisture product. 2. Results from batch 3 clearly demonstrate the stability of beta-anhydrous dextrose content at product moistures below 0.5% and mutarotation at moistures above 0.5%. 3. There was no change in beta-anhydrous dextrose content across the conditioning step at supply moistures below 2%. However, there may be a slight decrease at higher supply moistures. ( 4. There was no change in crystallinity across the 'conditioning step at supply moistures below 2%. There may i>e, however, a slight increase at higher supply moistures. 5. Products generally lost moisture with time and conditioned products remained at constant low moisture. EXAMPLE VIII A test was conducted according to the process described in Example III in a pilot plant assembled to allow the continuous concurrent operation of each of the processing steps. A 2-inch Readco was used in place of the 5-inch Readco. Cooling of the hot agglomerated Readco product prior to milling was done in a jacketed blender with a residence time variable from about 15 minutes to about 2 hours. The second conditioning step was accomplished during pneumatic transport cooling. Final product propertie were essentially the same as described in Example III. -17- </div>

Claims

<div class="application article clearfix printTableText" id="claims"> EXAMPLE IX The bulk handling properties of the crystalline dextrose product (hereinafter 'lCDP") were quantified using the Jenike Test Method. The results are compared to a commercial hydrate dextrose product known to haye acceptable handling properties, Data are summarized as follows: TABLE V Unconfined Yield Strength at a Consolidation Pressure of 520 Pounds per Square Foot (psf) Sample CERELOSE 2 001 CERELOSE 2001 CDP CDP Batch GU-317 MZ-394 9340 9332 Unconfined Yield Strength (Cake Strength*);47 46 36 28;a);Critical Rathole Diameter;Critical Rathole Diameter^ in Feet at Two Effective Heads;Sample Batch';CERELOSE 2001 GU-317;CERELOSE 2001 MZ-394;GBS 9340;CDP 9332;10 Ft.;2.6 3.0;2.7 2.2;15 Ft.;6.6 5.9 5.4 4.4;a) The less strength the better.;b) The smaller the diameter the better.;* pounds per square foot Having set forth the general nature and some specific examples of the present invention, the scope is now particularly set forth in the appended claims. -18- I V'iiiAT -WvVE CLAIM !3: A method of continuously making an anhydrous crystalline high dextrose bearing product from a concentrated starch hydrolyzate having a dry substance concentration of from 92% to 9 9% by weight comprising mixing said concentrated starch hydrolyzate while simultaneously seeding with a seed material selected from the group consisting of crystalline sugar and crushed crystalline dextrose.
2. The method of Claim 1 wherein mixing is conducted for from 1 minute to 1 hour.
3. The method of Claim 2 wherein the temperature of said hydrolyzate is maintained at 90°C to 135°C prior to mixing and at 80°C to 110°C during mixing.
4. The method of Claims 2 or 3 further comprising the step of milling said crystalline high dextrose bearing product.
5. The method of Claim 4 further comprising the step of screening the milled crystalline high dextrose bearing -> product.
6. The method of - Claim 4 further comprising the step of conditioning the milled "crystalline high dextrose bear- . ing product in a fluidized bed.
7. The method of Claim 6 wherein conditioning is conducted at a temperature from 65°C to 110°C for from- "7 minutes to 1 45 minutes followed by cooling to less than ■ 35°C. -19- "v. , - v> i C»f"'OOC f i A/wO
8. The method of Claim 6 wherein conditioning is conducted until the moisture content of said product is less than - 0.5% total moisture.
9. A method of continuously making a free flowing, handleable, composition stable, anhydrous high dextrose bearing product having less than 0.5% by weight total moisture from a concentrated starch hydrolyzate having a dry substance concentration of from • 92% to 99% by weight and a temperature from 90°C. to _ _• 135°C. consisting of the steps of mixing said concentrated starch hydrolyzate for from 1 minute to 1 hour at a temperature from 80°C. to- 110°C. while simultaneously seeding with a seed material selected from the group consisting of crystalline sugar, crushed crystalline dextrose and free flowing, handle-able dextrose to produce a crushed crystalline dextrose, milling said crushed crystalline dextrose, and conditioning the milled crystalline dextrose in a fluidized bed for from ■ . 7 minutes to 45 minutes at a temperature from 65°C, to 120,OC, followed by cooling to less than 35°C,
10. The method of Claim 9 consisting of the additional step of screening the milled crystalline dextrose prior to conditioning.
11. A continous method of making a free flowing, handleable, composition stable, anhydrous high dextrose bearing product having less than •„ 0.5% by weight total moisture frcm a concentrated starch hydrolyzate having a dry substance concentration of from 92% to \ 99% by weight and a temperature from 90°C. to . 135°C, consisting of the steps of mixing said concentrated starch hydro- yzate for a residence time from 1 minute to 1 hour t a temperature from 80 C, to 110 C, to produce crushed crystalline dextrose, 20 f -i- t' J O milling said crushed crystalline dextrose, and conditioning the milled crystalline dextrose in a fluidized bed for from 7 minutes to 45 minutes at a temperature from 65°C. to _ 12 0°C. followed by cooling to less than 35°C.
12. The method of Claim 11 consisting of the additional step of screening the milled dextrose prior to conditioning.
13. A free flowing, handleable, composition stable, anhydrous high dextrose bearing product having less than 0.5% by weight total moisture .prepared by mixing a concentrated starch hydrolyzate having a dry substance concentration of from 92 % to ■99% by weight for from 1 minute to - 1 hour at a temperature from 80°C. to 110°C. to produce a crushed crystalline dextrose, milling said crushed crystalline dextrose, and conditioning the milled crystalline dextrose in a fluidized bed for from 7 minutes to 45 minutes at a temperature from 65°C, to 120°C. followed by cooling to less than 35°C.
14. The product of Claim 13 vterein seeding with a seed material selected from the group consisting of crystalline sugar, crushed crystalline dextrose and free flowing, handleable dextrose is carried out simultaneously with mixing. - 21 - 1S7228
15. The product of Claim 13 or 14 wherein the concentrated starch hydrolyzate is at a temperature from 90°C. to •135°C. prior to mixing.
16. The product . cf claim 13 or 14 .wherein the milled crystalline dextrose is screened prior to conditioning.
17. The method of claim 6 wherein conditioning is conducted at a temperature from- , 65°C to 120°C for from 7 minutes to 15 minutes followed by cooling to less than - 35°C. ifCrc-aeuQAitg-c^- By H#?/thelr authorised Agents.^ A. J. PARK & SON. r- 22 - 20 </div>