NL8102644A - FREE-LIQUID CRYSTALLINE PRODUCT WITH HIGH DEXTROSE CONTENT. - Google Patents

Description

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Free-flowing crystalline product with high dextrose content.

The present invention relates to a free-flowing, manageable, crystalline, anhydrous product of high dextrose content, and in particular to a solid product of high dextrose content, which is stable in composition and does not form a cake after prolonged storage.

Solid dextrose is usually produced by crystallizing supersaturated high dextrose syrups and recovering the crystals in the α-dextrose monohydrate crystal form. This method is described in U.S. Pat. No. 3,039,935. Yields depend on carefully controlled cooling temperatures and the supersaturation conditions of the dextrose. Complete recovery of the dextrose from the syrup cannot be achieved by this method, since efficient crystallization of the dextrose and separation requires supersaturated dextrose solutions.

Thus, as the dextrose crystallizes, the solution is diluted and a significant portion of the dextrose remains in the syrup (the mother liquor) at the end of the dextrose crystallization step. Anhydrous α-dextrose is generally produced from the crystallized dextrose by dissolving its α-D-dextrose monohydrate crystals in water and crystallizing at temperatures 60-65 ° C in vacuum pans under carefully controlled process conditions.

It is known to produce this anhydrous α-dextrose from hydrolysates containing more than 96% dextrose on a dry matter basis (hereinafter referred to as "d.s.").

A method of affixing all solids in a conversion syrup without separating its dextrose has already been described in U.S. Patent 3,197,338, which discloses a method of preparing a crystalline non-cake forming dextrose pro- dumps. According to this patent, a purified conversion syrup with dextrose is concentrated to at least 95% d.s. (preferably more than 98% d.s.), crystallized by kneading at 77-110 ° C and extruded in the form of a strip or strand in a zone in which the product is rapidly cooled to 8102644-2 below 77 ° C. Then the extruded tape is crushed to a suitable particle size.

According to U.S. Pat. No. 3,236,687, the solids from a dextrose conversion syrup are converted into a solid form by subjecting a concentrated syrup having a dry matter content of 93-96% at 82-104 ° C to high shear in presence of gas, producing very fine glucose crystals. The product obtained is described as a seed containing creamy, foamy dextrose mass. This mass is dumped on a conveyor belt and secured in a number of cooling zones, in which lower temperatures prevail (e.g. the first zone at 82-104 ° C, the second zone at 60-82 ° C and the third zone below 38 ° C). The solidified mass is cut, conditioned at 49-82 ° C for two to three hours, ground and dried again.

A further known method for the production of granular dextrose involves a three-stage process in which a liquid hydrolyzate is contacted with seed material in a cutting or mixing device, followed by depositing the material on a continuous belt where it is cooled and turned into a solid slice. The slab is then crushed and sometimes undergoes additional treatment on a second continuous belt. This method is described in U.S. Pat. No. 3,650,829.

U.S. Pat. No. 4,059,460 describes a further process for the preparation of solid anhydrous dextrose. This method involves preparing a molten concentrated dextrose syrup with a d.s. concentration of 85-93% and a temperature above 110 ° C. The concentrate is mixed under shear and cooled to a temperature below 93 ° C to form a more viscous but still liquid dextrose mass. This liquid dextrose mass is concentrated at a concentration below 93% d.s. kept at a temperature above the crystallization temperature of dextrose hydrate. The mass is then shaped, rolled or deposited on a strip and converted into a solid mass. The solid mass is finally crushed and dewatered to an 81 0 2 6 4 4 * i t - 3 - water content of less than 2% =

Anhydrous dextrose products prepared directly from hydrolysates and other higher sugars in addition to dextrose in accordance with the prior art have generally been found to be unsatisfactory due to cake formation and handling problems. These products are difficult to transport in bags because of the tendency to form cakes. Moreover, these products cannot be mass-transported in cisterns, because of the poor flow properties, making unloading difficult if not impossible.

According to the present invention, the steps of mixing the liquid hydrolyzate, if necessary. with inoculum, conversion to a solid mass, and the crushing 15 performed in a single, continuous, heavy-duty mixer and thus efficiently combined into a single stage.

The product from this step is then conditioned to make it manageable and to provide composition stability.

A free-flowing, manageable, crystalline product of high anhydrous dextrose content is continuously prepared from a concentrated starch hydrolyzate. According to the method of the invention, the concentrated starch hydrolyzate is placed in a heavy-duty mixer (inoculum can be added optionally at this stage of the method), where it is converted into a crystalline form, crushed and cooled in a first stage. The crushed crystallized product is then further cooled and ground and can be sieved if necessary. Finally, it is crushed, ground and possibly. sieved crystallized product conditioned by drying to reduce the total moisture content.

The starch hydrolyzate to be used according to the present invention can be prepared by conventional methods, such as by enzymatic or acidic hydrolysis of starch. Concentration of the hydrolyzate to a d.s. concentration of about 92-99%, preferably about 95-99%, is then carried out by, e.g., evaporation in a film evaporator. This concentrate is referred to in the present description as "concentrated starch hydrolyzate".

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Concentrated starch hydrolyzate is placed at a temperature of about 90-135 ° C in a heavy duty mixer equipped with a cooling jacket to dissipate both heat for cooling and the exothermic heat of crystallization. Approx. 1-15% inoculum (d.s. basis) can be added at the same time if necessary or desired. Mixing is carried out for 1 min-1 h.

As a seed material, a crystalline sugar or previously prepared free-flowing, manageable product with high content of anhydrous dextrose can be used. The continuous process becomes self-grafting after a short working period and therefore grafting is not generally necessary.

Several heavy-duty mixers suitable for the present invention are commercially available. This includes Teledyne Readco's Readco Continuous Processor. Such devices are provided with cooling jackets for the removal of heat. The jacket temperature is maintained at about 20-40 ° C according to the present invention. A higher heat dissipation capacity can be obtained by means of a heat exchanger, which is connected in series with the heavy-duty mixing device. A conventional scraped surface heat exchanger, such as the VOTATOR R heat exchanger manufactured by Chemetron Corporation, is suitable.

Mixing the concentrated starch hydrolyzate and, if necessary. inoculum provides a crushed crystalline product which is dry and granular and typically has a particle size of powder up to about 50 mm in diameter.

Sufficient cooling is applied during mixing to provide a crushed product at a temperature of about 80-110 ° C.

The crushed crystalline product is then preferably cooled to below about 30 ° C. This can be done, for example, in a jacketed mixer, through which cooled conditioned (i.e. with low humidity) air is blown. Then, the cooled crystalline product is ground by conventional means to a reduced particle size 8102644 = 4 * - 5. Sieving is only necessary if a specific particle size is required.

It was crushed, ground and possibly. sieved crystalline product is then conditioned in two stages. In the first stage, a fluidized bed is used, in which the crystallized product is fluidized for a residence time of about 17-45 min, preferably about 7-15 min, at a temperature of 65-120 ° C, whereby a product is obtained with a total moisture content of less than 0.5%. 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 according to the present invention by either a treatment in a second fluidized bed or during pneumatic transport, preferably using dehumidified air in both cases. Other types of conditioning devices, which achieve the same reduction in humidity, can be used. The final conditioned product with a high dextrose content is excellent in handling and has excellent compositional stability.

Various properties of the product according to the invention can be measured. These are the dextrose content, the moisture content, the anhydrous α and β-dextrose content, the crystallinity, the particle size and the handling properties. The results of these measurements are reported in the examples of the description.

The dextrose content can be measured by conventional HPLC (high pressure liquid chromatography). Moisture content and particle size can also be measured in the known ways.

The product is anhydrous because of the elevated temperatures used in the conversion. More than about 50% of the product is in the anhydrous fr form and the remainder in the anhydrous α form, due to the conversion at the low humidity and high speed. The respective fractions of the anhydrous α and β dextrose are determined by NMR (nuclear magnetic resonance).

The crystallinity is a measure of the crystalline, or non-amorphous, structure of the product. The crystal linearity is determined from the melting heat measurements with a DSC (differntial scanning calorimeter). Samples of anhydrous α-dextrose prepared by classical crystallization were used as a standard for fully crystalline material. The crystallinity of the product was determined by comparing the melting heat of the product with that of a crystalline standard with the same percentage of α- and 3-dextrose as that of the sample. This corrects for the difference in heat of fusion between anhydrous a- and β-dextrose.

The handling of the product is expressed by the Jenike test method, a laboratory method, which quantifies the flow and storage properties of solid masses. (See "Know Your 15 Material - Hów to Predict and Use the Properties of Bulk Solids," Chemical Engineering / Deskbook Issue, JR Johanson, Oct. 30, 1978, and "Flow Properties of Bulk Solids," ASTM, Proc., Vol. 60, 1960, 1168-1181. Test results for the product are compared with the results for lipidated α-dextrose prepared by classical crystallization.

Experiments were performed with a DSC and SEM (scanning electron microscope) to subjectively test the handling of the product of the present invention and of a typical product of a conveyor belt conversion process, which very strongly exhibited the tendency to form cakes. compare. The product of the present invention had a higher, more defined crystal structure and a better dispersion of the amorphous phase, compared to the assembly line product. Both of these factors are believed to contribute to the excellent handling properties of the product of the present invention.

The invention is now further illustrated by the following examples.

EXAMPLE I

Starch hydrolyzate was concentrated to at least 90% d.s. using a film evaporator (except in Run No. 1 in Table A, where a syrup was used, which was 81 0 2 6 44 * i - 7 - prepared by dissolving crystalline anhydrous dextrose followed by concentration to 85.3% ds in a film evaporator). Subsequently, concentrated starch hydrolyzate was converted to a solid in several batchwise runs using a jacketed mixer, fitted with double arms and overlapping sigma blades, manufactured by Teledyne Readco. The mixer consisted of a rectangular trough with a curved bottom, which formed two longitudinal half cylinders and a saddle. The mixer was equipped with two blades of the sigma type, which rotated together with overlapping rotation circles. The mixer had a working capacity of 5.7 l and a total capacity of 8.5 l. Conditions and results are shown in Table A.

Anhydrous dextrose was used as the material for Runs 3, 4, 5 and 6. In Run 1, no inoculum was used. The product from Run 1 was used as the material for Run 2. The batch mixer was overfilled in Runs Nos 1 and 2, preventing the stirrers from ensuring efficient kneading and shearing of all 20. Higher sheath temperatures in these tests also contributed to longer conversion times. When the batch was reduced to about 4 kg and the jacket temperatures to about 60 ° C, the conversion time was significantly reduced. The crystalline dextrose products tended to form cakes.

EXAMPLE II

A continuous process was performed in a Readco Continuous Processor manufactured by the Teledyne Readco Company. The mixing chamber was 0.914 m long and consisted of double cylindrical chambers with a diameter of 127 mm. Two parallel stirring shafts rotating in the same direction were used in the device. The blades of one of the stirrers were lenticular and just did not touch the walls of the chamber or the second stirrer, which was 90 ° out of phase 35 with the first. This not only ensured sufficient mixing, but also a self-cleaning effect of the stirring blades. The entire chamber was jacketed to cool the material to be mixed. The feed time of the hydrolyzate 8102644

9 C

- 8 - each continuous run averaged 5 min. The results of some early run trials are listed in Table B.

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The feed in Runs No. 5-9 was dissolved anhydrous dextrose. In all tests, crystalline anhydrous dextrose was the inoculum. The crystalline dextrose. product showed tendency to cake.

EXAMPLE III

A sample was prepared using all of the method steps of the present invention.

A 127 mm diameter Readco Continuous Processor was used, followed by grinding and conditioning in a fluidized bed consisting of a single tube with a diameter of 76 mm and a height of 1.52 m. The product analysis and the particle size distribution of the unscreened product were as follows:

PRODUCT ANALYZES

15 d.s.,% 99.6 dextrose,% d.b. 98.2 anhydrous 3-dextrose,% d.b. 51.1 crystallinity,% as is 92 color (40 ° Be) 1.1, 20 as (SO4),% d.b. 0.01

SCREEN ANALYSIS

particle size distribution 0.84 0.42 0.250 '0.149 0.105 0.074 <0.074 mm 6.8 25.4 22.0 14.6 12.4 1.8 16.0% 25 The Readco Processor was run for a little longer than an hour production speed of approx. 2.17 kg / min. started without the use of inoculum. The product from the Readco Processor consisted of hot, agglomerated material up to a size of about 50 mm. This material was spread out and left to cool for about 1 h and then ground in a single step with a Fitz mill. The ground product was first conditioned in the fluidized bed with a residence time of about 15 min at 65 ° C to reduce the total moisture content to less than ca.

0.5 S. This treatment was followed by a second step through the fluidized bed under conditions such that the final product was cooled to below 35 ° C.

8102644, 12- t

A portion of the sample was used to fill a 45 kg three-layer polyethylene bag. The saw was then placed under five bags, each containing 45 kg anhydrous dextrose, to mimic the weight in stack transport. After 37 days, the bag was opened and the sample material, which could be called a "soft aggregate". I.e. that chunks could easily be broken by hand.

EXAMPLE IV

A number of samples were prepared according to the complete procedure as described in Example III, at different dextrose levels. The product analyzes were as follows: anhydrous test dextrose moisture B-dextrose crystallinity ash no.% Dvb. % ''% d.b. % as-is_% d.b.

1 98.7 0.2 67.5 93 0.01 2 98.1 0.3 61.8 89 0.02 3 94.6 0.8 66.7 62 0.37 20 4 93.8 0.5 70.2 73 0.02

In each run, a 45 kg sample was placed in a bag similar to Example III. All bags were then stored under twenty bags, each containing 45 kg of dextrose, in a factory warehouse. After more than two months, the bags were inspected and it was found that no more than a soft aggregate had developed. The product from Run 3, which had a moisture content of 0.8% (inadvertently above the desired upper limit of about 0.5% moisture), was slightly caked compared to the other three. formed.

30 EXAMPLE V

A number of conditioning tests were conducted to impart handling (making anti-caking properties) to the products prepared according to the method described in the previous examples. The conditioning was performed in a 76 mm fluidized bed. The process temperatures were obtained with hot water or steam jacketed around the fluidized bed. The fluidizing air was fed through a 28 hole bottom distribution plate 8102644-13 with a diameter of 1.6 mm at an operating fluidization velocity of 0.61 m / s (21 ° C, 1 at). The results are reported in Table C.

EXAMPLE VI

Two samples were prepared according to the complete procedure described in Example III. The hydrolyzate supplied contained 95.9% d.b. dextrose. The product from the Readco Processor for the first sample had a content of 98.9% ds, a crystallinity of 74% as-is, and a water-free β-dextrose content of 57.7% ds, and for the second sample a content of 98.9% ds, a crystallinity of 73% as-is, and an anhydrous dextrose content of 61.9% d.Sc. The first sample was conditioned in a fluidized bed at 99 ° C for 18.6 min. after which a conditioned product with a content of 99.6% ds, a crystallinity of 77% as-is, and an anhydrous β-dextrose content of 58.5% db was obtained. The second sample was conditioned in the fluidized bed at 118 ° C for 7.7 min, after which a conditioned product with a content of 99.6% ds, a crystallinity of 74% as-is, and an anhydrous β-dextro- a content of 63.3% was obtained.

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The conditioning results are mainly limited to a decrease in the total moisture content. No noticeable changes in the final product composition (anhydrous 3-dextrose and crystal-5 linearity) occurred.

EXAMPLE VII

Tests were conducted to determine the influences of moisture, storage temperature and storage time on the crystallized dextrose products. Crystallinity levels of both conditioned and unconditioned products were also determined.

Three test batches were prepared. Each batch was prepared using a Readco Continuous Processor, yielding a product with different moisture content (3.6%, 1.9% and 0.9%). The product of each series was split into two parts and treated as follows: 1. One part was simply stored at ambient temperature.

2. The second part was conditioned in a fluidized bed on the day of production.

All products were analyzed immediately after manufacture and then again at the intervals listed in the table. The results are listed in Table D.

25 'TABLE D

anhydrous batch sample, analyzes, moisture 3-dextrose cry. no. description 3 'after days%% d.b. % as-is 1 product 0 3.6 53.7 85 25 "13 3.7 * 12.0 - 31 6.3c; 7.2 conditioned product 0 0.4 50.3 92 13 0.4 47.6 30 B 31 0.3 49.8 2 product 0 1.9 61.8 87 n 14 1.7 9.8 "32 1.5 8.9 conditioned 35 product 0 0.3 61.0 86 13 0.3 58.5 - 31 0.3 60.4 8102644 • r ν - 16 - TABLE D (continued) anhydrous batch sample * analyzes, * moisture g-dextrose cry. no description} after days 0 '%% d.b. % as-is 5 3 product 0 0.9 62.6 82 "14 1.2 21.1" 27 0.8 24.5 conditioned product 0 0.3 61.2 84 10 "14 0.4 64.6 "27 0.4 65.2 a) All samples were prepared in the same Readco Continuous Processor with a throughput of about 2.17 kg / min without inoculum. The product temperatures for batches 1, 2 and 3 were 91 ° C, 93 ° C, respectively. 99 ° C.

b) Number of days between analysis and sample preparation.

c) This high moisture content is an aberration.

From the above results, the following conclusions were drawn.

1. There were no noticeable differences in the anhydrous 3-dextrose contents of the starting products depending on the moisture content. The small differences can probably be attributed to mutation rotation before the analysis of the higher moisture product.

2. The results of batch 3 demonstrate the stability of the anhydrous β-dextrose content at 30 moisture levels of the product below 0.5% and of mutation rotation at moisture levels above 0.5%.

3. No change occurred in the anhydrous β-dextrose content during the conditioning step at moisture levels of the feed material below 2%. At higher moisture contents of the feed material, however, a slight decrease may occur.

4. No change in crystallinity during the conditioning step occurred at moisture levels of the feed material below 2%. However, at higher moisture contents of 81 02 6 44% - 17 - the feed material may slightly increase.

5. The products generally lost moisture over time and conditioned products maintained a consistently low moisture content.

EXAMPLE VIII

A test was carried out according to the method described in Example III in a pilot plant, arranged so that each of the process steps could be run continuously side by side. A 51 mm Readco was used instead of the 127 mm Readco. The cooling of the hot agglomerated product from the Readco prior to grinding was carried out in a jacketed mixer with a residence time ranging from about 15 min to 2 h. The second conditioning step was performed by cooling during pneumatic transport. The properties of the final product were essentially the same as described in Example III.

EXAMPLE IX

The mass handling properties of the crystalline dextrose product (hereinafter "CDP") were quantitated using the Jenike test method. The results were compared to a commercially hydrated dextrose product, which is known to have acceptable handling properties. The following data were obtained:

TABLE E

2 open yield strength after a hardening pressure of 2550 kg / ma) open yield strength sample batch (cake strength *) 30 CERELOSE 2001 GU-317 220 CERELOSE 2001 MZ-394 215 CDP 9340 176 CDP 9332 137 35 81 0 2 6 44 * - 18 - TABLE E (continued) critical rat hole diameter critical rat hole diameter ^ in mm at 2 effective 5 sample charge trough diameters 3 m 4/5 m. CERELOSE 2001 GU-317 793 2013 CERELOSE 2001 MZ-392 915 1800 CDP 9340 824 1647 10 CDP 9332 671 1342 a) The lower the strength, the better.

b) The smaller the diameter, the better.

* kg / m2.

15 8102644

Claims (17)

Process for the continuous preparation of high-dextrose crystalline product from a concentrated starch hydrolyzate with a solids concentration of 92-99% by weight, characterized in that the concentrated starch hydrolyzate is mixed together while it is inoculated simultaneously with a seed material from the group of crystalline sugar and crushed crystalline dextrose. 2. Process according to claim 1, characterized in that the mixing is carried out for 1 min to 1 h. 3. Process according to claims 1-2, characterized in that the temperature of the hydrolyzate is kept at 90-135 ° C before mixing and at 80-110 ° C during mixing. 4. Process according to claims 1-3, characterized in that the crystalline product with a high dextrose content is also ground. 5. Process according to claims 1-4, characterized in that the ground crystalline product with high dextrose content is also sieved. 6. Process according to claims 1-5, characterized in that the milled, crystalline product with high dextrose content is conditioned in a fluidized bed. 7. Process according to claim 6, characterized in that the conditioning is carried out at a temperature of 65-120 ° C for .7-45 min, followed by cooling to below 35 ° C. A method according to claim 6, characterized in that the conditioning is continued until the moisture content of the product is less than 0.5% total moisture. 9. A process for the continuous preparation of a free-flowing, manageable, anhydrous product with a high dextrose content, which is stable in composition and contains less than 0.5% total moisture, from a concentrated starch hydrolyzate with a concentration of 8102644-20. of dry ingredients of 92-99 wt. % and at a temperature of 90-135 ° C, characterized in that the concentrated starch hydrolyzate is mixed together for 1 min to 1 h at a temperature of 80-110 ° C, while simultaneously being inoculated with a seed material from the group of crystalline sugar, crushed crystalline dextrose and free-flowing, manageable dextrose to form a crushed crystalline dextrose; that the crushed crystalline dextrose 10 is ground; and the ground crystalline dextrose in a fluidized bed for. The mixture is conditioned for 7 -45 min at a temperature of 65-120 ° C, followed by cooling to below 35 ° C. 10. Process according to claim 9, characterized in that the ground crystalline dextrose is also sieved prior to conditioning. 11. Continuous process for preparing a free liquid, manageable, anhydrous product of high dextrose content, which is stable in composition and contains less than 0.5% total moisture, from a concentrated starch hydrolyzate with a concentration of dry ingredients of 92-99% by weight and at a temperature of 90-135 ° C, characterized in that the concentrated starch hydrolyzate is mixed together for a residence time of 1 min to 1 h at a temperature of 80-110 ° C, to form a crushed crystalline dextrose; that the crushed crystalline dextrose is ground; and the ground crystalline dextrose in a fluidized bed for. The mixture is conditioned for 7-45 min at a temperature of 65-120 ° C, followed by cooling to 35 ° C. A method according to claim 11, characterized in that the ground dextrose is screened prior to conditioning. 13. Freely liquid, manageable, anhydrous high dextrose product, which is stable in composition and contains less than 0.5% total moisture, prepared by a concentrated starch hydrolyzate having a dry matter concentration of 92-99% by weight for 1 min 8102644 «É- '-T?" - 21 - up to 1 h at a temperature of 80-110 ° C by mixing together, to form a pulverized crystalline dextrose; by grinding the pulverized crystalline dextrose? And by the ground condition crystalline dextrose in a fluidized bed for 7-45 min at a temperature of 65-120 ° C, followed by cooling below 35 ° C. 14. A composition according to claim 13, characterized in that the seeding is simultaneously inoculated with a seed material from the group of crystalline sugar, crushed crystalline dextrose and free-flowing, manageable dextrose. 15. A composition according to claims 13-14, characterized in that the concentrated starch hydrolyzate has a temperature of 90-135 ° C prior to mixing. Composition according to claims 13-14, characterized in that the ground crystalline dextrose is sieved prior to conditioning. Method according to claim 6, characterized in that the conditioning is carried out at a temperature of 65-120 ° C for 7-15 min, followed by cooling below 35 ° C. 81 02 6 44