DE1951460C - Agglomerated sugar product - Google Patents

Description

Crystalline sugars used in the food and drug industries are generally of two main types. The first type is sucrose made from sugar cane or sugar beet. The second type is Dextrose, which is generally obtained by hydrolyzing starch to monosaccharide.

Because sugar in crystalline form is required by the food and drug industries, the crystallization of the uncrystallized raw sucrose or dextrose is apparently a necessary extraction process. The art, therefore, has developed many methods that have become common for the crystallization of raw sugar. One of the most common of these methods is to concentrate a uncrystallized raw sugar in solution to penetrate, AAnn uie solution iu a uucisättigten state and then to seed the supersaturated solution with crystals already formed sugar. When the solution is then cooled, new sugar crystals form and grow. After the crystals have formed, the remaining mother liquor is separated off from the crystals. The crystals are then washed and dried to obtain the finished crystalline sugar.

The food and drug industries require crystalline sugars for many reasons is agglomerated. One of the many areas in which crystalline sugar is requested is in manufacturing edible tablets. The term "edible tablets" is well understood in technology, and it is used here used in their usual meaning. Examples of edible tablets include: candies, peppermint tablets, medical pills and placebos.

Agglomerated crystalline sugar is generally made by first making a crystalline Sugar is produced according to the method just described with the modification that before Drying or, if dry sugar is present, after moistening, an agglomerating agent to the Sugar is added. The sugar is then agglomerated by conventional methods, e.g. B. at increased Temperatures using a granulator then dried and as an agglomerated granulated sugar product sold or consumed.

Up until now it was mostly common to use either a liquid sugar (e.g. a Sugar solution) of the agglomerated type or a syrup, e.g. B. corn syrup to use. For example for agglomeration of crystalline dextrose, a liquid solution of either dextrose or of Corn syrup is generally used as an agglomerating agent.

The technical usefulness of an agglomerated sugar is heavily dependent on the degree of its resistance to caking, its flowability, the agglomerate strength, its low level of dust, but also on its ability, when used for the production of edible tablets, to form a strong, easily compressible tablet of the desired density. In general, for any agglomerated sugar, it is believed that the size of the agglomerate particles plays an important role in achieving acceptable sizes of these desirable properties. For many types of agglomerated sugar, for example, the following applies: if the diameter of the agglomerated particles decreases, the losses in terms of tablet breakage and dusting increase accordingly. and production decreases. Furthermore, with this and other types of agglomerated sugar, as the diameter of the agglomerated particles decreases, the weight and volume of a tablet increases, resulting in a loss of compressible at constant full volume. The problem of dusting, disintegration and compression can therefore generally be minimized for any system using a particular agglomerating agent to form edible tablets therefrom if the agglomerated particles are then relatively large, usually greater than 200M: krones, and preferably greater than 400 microns. - usual

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of the agglomerated sugar particles from the sieve a mesh size of 65 or more (mesh number below 65) is collected, then the agglomerated Sugar properties on. which are particularly desirable for tablets.

With the previous use of conventional agglomerating agents Agglomerate properties and properties have become acceptable levels of sieving behavior of the edible tablets only with difficulty and with the use of large amounts of agglomerating agents and get water. Sometimes, for example B. when sucrose or mixtures of sucrose and dextrose should be agglomerated, the aggomeration failed either completely, or only rarely were the agglomerates more acceptable Quality and were generally not reproducible. In many cases when dextrose was agglomerated, the agglomerated product formed was only of poor quality. Such results are apparently a real problem relevant to the whole ·; Industry.

The object of the invention is. this industry with new agglomerable products of dextrose, sucrose and / or mixtures of dextrose and sucrose, which contain an agglomerating agent, and with agglomerated sugars and tablets made therefrom, all of which are acceptable and are mostly of improved quality, and which products the mentioned technical problems eliminate or significantly reduce.

Part of the solution to this problem is the creation of a crystalline sugar product in agglomerated form Form, which can be easily tabletted, and its crystals are extraordinarily strong and new Binders for use in the production of agglomerated crystal sugar are well suited.

According to the invention, this object is achieved in that the conventional agglomerating agents used hitherto be replaced by an agglomerating agent, commonly called a low dextrose equivalent starch hydrolyzate (hereinafter referred to briefly as D. E.) can be designated. By using this Hydrolysates can be made into new types of agglomerated sugar and edible tablets.

The invention relates to an agglomerated sugar product for the production of edible tablets, which is characterized by a crystalline sugar, possibly an addition of citric acid, magncsium stearate and an artificial flavoring agent, 1 to 10 percent by weight of a starch hydrolyzate as Agglomerating agent produced by enzyme and / or acid treatment of a starch source and a dextrose equivalent of 5 to 25 and one

descriptive ratio of 2.0, where the Descriptive ratio is the sum of the percentages of sugars with degrees of polymerization from I to 6 divided by the dextrose equivalent means

This combination forms in the presence of sufficient water and subsequent drying an agglomerate. Due to the presence of the hydrolyzate, the crystalline sugar easily agglomerates Use of conventional agglomeration processes with the formation of a crystalline sugar agglomerate strong particles, which has excellent sieving properties and flowability, and which on storage and transportation shows less breakage and dusts than usual sugar agglomerates.

Crystalline sugars useful in the invention include all types of crystalline sugar products. such as B. Dextrose. Sucrose. Lactn «» mu < ka; ^ u "^ gen from it. Many of these types of sugar are known in the art and are commercially available items under various trademarks. Such types of sugar are generally produced and crystallized by conventional methods.

The crystalline sugars which can be used according to the invention can either be in dry or in wet form mixed with the agg! omerizing agent will. Preferably the crystalline sugar used is one which is in its centrifuge cake pan located after its crystallization, which cake is washed and adjusted to a water content only the water of hydration was thrown, which, ν ^ nn present. 1 to 16% de> cake weight is. Most of the time this is done in this cake is sufficient water to ei κ- necessary amount of water to agglomerate the To provide sugar. This necessary amount of water fii; the agglomeration of the aforementioned according to the invention Product, excluding the hydration scientist, is generally 1 to about 8 percent by weight of the entire product.

As already mentioned, the agglomerating agent used according to the invention can generally be defined are called low D.E. starch hydrolyzate. These hydrolyzates are applied in an amount vim 1 to about 10 weight percent of the sugar solids and preferably from 2 to about 4 percent by weight.

The starch hydrolysates used according to the invention for the production of crystalline sugar agglomerates from low D. E. are a relatively new genus Starch material. These starch hydrolysates are prepared in that a starch source of an enzyme or Acid treatment or a combination of both. It is important that the starch hydrolyzate a relatively low D.E. of less than 25 and preferably a D.E. in the range from 5 to 25. The preferred materials have a D.E. within the range of! 0-15. Such starch hydrolysates have been found to be excellent agents for increasing moisture absorption Normally hygroscopic foods decrease while using other hydrolysates of a D.E. which is significantly outside this range leads to inferior products. which still show a tendency. Absorb moisture, and therefore to cake tend or get sticky.

The term DE is used herein to refer to the reducing sugar content of the dissolved solids in a starch hydrolyzate, expressed as percent dextrose.

The starting starch, which is subjected to the hydrolysis treatment, can come from a wide variety of starch materials, such as. B. Cereal starches. Wax starches and / or root starches. Typical door these groups are corn, potato. Tapioca, grain sorghum, waxy milo, waxy maize and rice starch. As used herein, "starch hydrolyzate" includes hydrolyzed starch materials from a wide range of known starch sources.

As mentioned earlier, those are preferred for the In the invention, starch hydrolysates used are those with a D.E. between 5 and 25, which can be produced by any desired method.

In the case of a process A designated in Example 1

treated with a single enzyme preparation of bacterial alpha-amylase. This is an aqueous Slurry of waxy starch with a solids content below 50% of the hydrolysis action of bacterial alpha-amylase subjected under suitable fermentation conditions to obtain a starch hydrolyzate. The hydrolyzate can also be characterized by the fact that it is the sum: in percentages (dry basis) Saccharides with a degree of polymerization of 1 to 6 divided by the D. E. possesses to a larger To give ratio as 2.0. This relationship is called the characteristic or descriptive relationship designated. Those low D.E products with a descriptive ratio less than 2 are something undesirable because, for example, they have less water solubility and also tend to be cloudy Form in solution compared to products with a ratio of at least 2.

The same product as described above can also be manufactured in other ways. For example A mixture of starch and water with a solids content below 50% can first have the hydrolysis effect a bacterial alpha-amylase followed by a high temperature heating step to solubilize any undissolved starch. Because this temperature tends to it is then necessary to inactivate the enzyme.

to cool the solubilized partial hydrolyzate and a second hydrolysis by treatment with additional to bacterial alpha-amylase to obtain the final starch hydrolyzate. This The procedure is referred to as method B in example 1.

A third method of making the preferred class of low starch hydrolysates D. E. .. referred to as method C in example 1, consists in a mixture of starch and water through Hydrolyze exposure to acid to produce a D. E.

between 5 and 15. The partial hydrolyzate is then subjected to the action of bacterial alpha-amylase in order to use a starch hydrolyzate a D.E. from 10 to 25 to win.

A starch hydrolyzate particularly preferred for the invention has the following characteristics: water content at most 5% and a D.E. from 10 to 13. As already indicated, the agglomerated Products preferably formed by adding a dry agglomeration to wet crystallized sugar

⁶ S merier from starch hydrolyzate of low DE is added. Although this method is preferred, other methods of forming it can be used. For example, the agglomerating

Low DE starch hydrolyzate can first be placed in a solution containing up to 60% solids with enough water to provide 1 to 16 weight percent water in the finished agglomerated products. This solution can then be added to dry granulated sugar with mixing or spraying. Instead, the agglomerated product of the present invention can be formed in situ by mixing water, dry granulated sugar, and the dry agglomerating agent with moisture as low as 2%.

Regardless of the method by which they are obtained, the agglomerable products of the invention are easily made using more conventional ones

Methods agglomerated. The agglomerated f roauKie thus formed naoen excellent screening behavior, not cake, have flow and contain strong agglomerated particles which do not dust and not get broken. Furthermore, the agglomerated products have high bulk density and compressibility and can therefore be easily made into strong, edible tablets using conventional methods.

In a typical example of the invention and its application, an agglomerated product was thereby formed formed that 97 parts by weight of wet dextrose crystals and 3 parts by weight of a starch hydrolyzate of IOD. E. Were mixed, the water content of the mixture was between 2 to 4 percent by weight excluding the water of hydration. The mixture was then passed through an agglomerator (e.g. a Colton granulator) and dried.

The crystalline agglomerates came out of the dryer with the usual water contents. The agglomerates were found to be of a hard crystalline nature. When subjected to pressure, e.g. B. in a conventional tablet machine, the agglomerates only require about half the normal pressure, such as it is generally required to form a strong tablet.

Articles made in accordance with the invention include all types and shapes of pressed or extruded Fgglomerated sugar products. The base composition of these products comprises an agglomerated sugar un ^«1 a starch hydrolyzate of low DE In the case of placebo no further addition in the tablet or pill is generally present.

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and candy cigarettes can contain common flavors, like citric acid or Ch! "ophyil added will. For medical pills, Jie is concerned Medicine, vaccine or antibiotic added in the usual dose.

The agglomerable compositions according to the invention and agglomerates have many uses in the food and drug industries. Apart from their usefulness in the aforementioned manufacture of edible tablets they use in other areas, e.g. B. those where rapid dispersibility in water, uniform coarse particle size, security against breakage and dust is desirable.

The following specific examples illustrate the invention without restricting it. All in it percentages given are by weight.

fied

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go al

Time c

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W (was alpha starch suitable for i Amy der ^ Kon erha!

sated. received

example

The following specific procedures illustrate the three basic methods of manufacture already mentioned of starch hydrolysates of low D.E. which are used as agglomerating agents according to the invention.

Method A - one step enzyme process

An aqueous starch slurry was prepared containing 30 weight percent solids from waxy milk starch. The temperature of the pulp was increased and held between 85 and 92 ° C. A bacterial alpha-amylase preparation was added in an amount just above 0.025 percent by weight of the starch over a period of a little over 30 minutes. The mixture was then held at the same temperature for a further 30 minutes. The temperature was then ^{lowered to less than 80 °} C. and the conversion was allowed to proceed until the desired DE was reached. The temperature of the mixture; was then suddenly increased to over 120 ^° C. in order to inactivate the enzyme and to terminate the conversion.

The following table I shows typical saccharide analyzes of hydrolysates obtained according to the method of low DE DP denotes the degree of polymerization. DP ₁ represents the total amount, expressed in percent by weight, dry basis, of monosaccharides present in the hydrolyzate. DP _{2 represents} the total amount of disaccharides present in the hydrolyzate, etc.

Table I.
Typical saccharide analyzes

Hydrolyzate composition

DP ₁

DP ₂

DP ₃

DP ₄

DP ₅

⁵⁵ DP ₆

DP ₇ and higher ..

Total DP; -> 6
6o

Descriptives
Ratio ....

0.1
1.3
1.8

1.8
1.8

3.3
89.9
10.1

2.0

10

0.3

3.4

4.3

3.5

3.6

7.0

77.9

22.1

2.2

D.E. 15th

0.7
5.5
6.9

5.2

5.5

10.6

65.6

34.4

2.3

20th

1.4 7.6 9.4

6.9

7.4 14.3 53.0 47.0

2.4

25th

2.4

9.7

! 2.0

8.6

9.3

18.0

40.0

60.0

2.4

Method B - two-step enzyme process

Unmodified corn starch was slurried in water, U.N. an aqueous suspension with a

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Content of 28 to 32 percent by weight of the unmodified To yield cornstarch. The pH was set to 7.5 bi <; 8.0 set. To this mixture became bacterial alpha-amylase added in an amount of 0.05% based on the starch solids. This Starch suspension was brought to a temperature of 90 to 92 "C over a period of 30 minutes held container added with stirring. After completion of the addition of starch, the liquefaction continued for 60 minutes, after which time the hydrolysis was within a D.E. range from 2 to 5. The liquefied starch was then heated to and at 150 ° C held for 8 minutes. The heat treatment destroyed the remaining enzyme activity and led to reduced yield losses in the filtration.

Further saccharification to the final DE was effected by adding more bacterial alpha-amylase after cooling the liquefied starch hydrolyzate to a temperature suitable for conversion. The liquefied starch was ^{cooled to 80 to 85 °} C. and bacterial alpha-amylase was added in an amount of 0.02 percent by weight of the starch solids. After a conversion time of 14 to 20 hours, the desired final DE was obtained (20).

The finished starch hydrolyzate product was analyzed and the following analytical values were obtained receive.

table

DP, DP ₂ DP ₃ Table II DP ₅ dp " DP ₇ , Descriptives
ratio D.E. 2.4 7.5 10.8 DP, 6.8 15.1 49.4 2.4 20.7 8.0

Method C - two-step acid-enzyme process

Different samples of corn starch (A, B and C were slurried in water to obtain pulps with Baume ranges from 14 to 22 °. These pulps were partially hydrolyzed with acid to the highest; 15 DE The respective DE, which was produced by acid hydrolysis in each case the pattern obtained can be found in Table III.After acid hydrolysis, the slurry was neutralized to a pH between 6 and 7. The neutralized liquid was cooled to 80 bis: 85 ° C and treated with bacterial alpha-amylase in an amount as indicated below A final DE "or 19 to 21 was obtained for each of the samples in a time between 1 and 3 hours. The final converting fluids are faintly colored. These fluids are slightly refined and evaporated to 42 ° trees to give syrups resulting dry products can also be obtained. Tables III and IV give the reaction conditions for the conversion and the product analyzer.

Enzyme Conversion Conditions

sample DE des
Acid hydrolyzate Dry matter temperature
C. PH Enzyme dose time
hours End-D. E. A.
B.
Q 15.2
12.9
10.3 38
37.5
38.1 80
'85
85 6.5
6.5
6.5 0.01
0.05
0.1 1
2
2 19.7
20.2
21.8

Table IV Product Analysis

sample End-D. E. Dry
substance DP, DP, DP, DP ₄ DP ₅ DP ₆ DP ,, Descriptives
ratio A. 19.7 72 3.9 5.8 8.2 12th 7.3 10.2 57.4 Zl B. 20.2 72 Z3 5.9 8.5 6.4 6.6 12.6 57.7 Zl C. 2 », 8 75 Z3 8.3 10.9 8.1 9.2 16.9 44.3 2.5

Example 2 Production of crystalline dextrose agglomerates

A starch hydrolyzate with a D.E. of approximately 10 was prepared by following the procedure of Example 1, Method A. Analysis of this product was essentially the same as the analysis of the 10-D. E. Product in Table I. Two approaches Centrifuge cake sugars, crystalline dextrose, each weighing 22.7 kg, were mixed with the hydrolyzate, the hydrolyzate in an amount from 2 to 4 weight percent solids was added and either dry or with a small amount Amount of water as indicated in Table V was used.

The original centrifuge cake before the

Additive hydrolyzate contained 12 to 15% water, worii 9% Hydratiocswasser is included according to the

Mixing the dextrose with the hydrolyzate voi

low D.E. during 10 minutes in a common

Mixing machine was the mixture in a hot air Rotary dryer with steam jacket of one temperatu

of 132 ° C transferred. After 15 minutes dry The dry product was cleaned using a:

Tyler No. 10 sieves sighted and the percentage « Throughput viewed as yield (i.e. as product) The agglomerated products had the in labeile, λ

specified sieve ratios.

For purposes of comparison, the same basic procedure as described was carried out again

ίο

the amendment that instead of using the hydrolyzate of low D.E., customary and comparable Amounts of common agglomerating agents were used, namely liquid dextrose and corn syrup (60% solids). Three different types of corn syrup were used. Additionally An experiment was carried out with complete omission an agglomerating agent. This trial is considered a control and is "with run 1

designated. Another experiment was carried out with the addition of only 2% water to the kuchei without any addition of agglomeration agents (batch 16).

For comparison purposes, Table V includes screen performance and other properties of these more common Agglomerates. For the sake of simplicity, the hydrolyzate is in the table as HY and the liquid dextrose referred to as LD.

Table V approach additive no crowd water A.I.) Over 14 ") Sieve content% flow rate: 20th 35 42 60 80 IfX) Corn Syrup A size 99.6 98.8 90.4 86.6 73.8 38.4 18.0 1 Corn Syrup A - 8.9 82.4 % 99.6 98.2 86.8 77.4 39.2 16.6 1.2 2 Corn Syrup A 2% 8.1 68.8 4.0 97.2 91.4 62.4 47.8 12.6 0.8 0.4 3 Corn Syrup B 4% 7.6 46.8 5.0 71.6 38.2 3.0 1.4 0.4 0.0 (). () 4th Corn Syrup B 6% 9.4 11.4 10.0 99.0 96.8 74.4 62.6 25.8 3.6 0.8 5 Corn Syrup B 2% 8.4 39.4 24.5 96.6 86.4 49.2 33.4 11.4 2.4 1.0 6th Corn Syrup B 4% 8.8 38.0 4.5 91.0 60.0 20.0 11.8 4.0 1.2 0.4 7th HY 6% 8.5 28.0 13.0 82.2 60.4 26.4 18.6 6.4 1.4 0.8 8th HY 8th% 5.9 37.2 40.0 98.8 95.6 71.4 60.4 32.8 7.8 2.6 9 HY 2%
trnclcen 8.6 46.2 69.0 97.4 93.6 71.8 59.0 26.0 5.0 2.0 10 HY Ll L / WVwi J
4%
dry 7.1 60.8 7.5 99.0 95.2 66.2 57.0 30.6 8.2 3.2 Il Corn Syrup C 2%
wet 8.3 44.0 13.0 96.8 86.6 54.2 42.2 20.2 5.6 2.4 12th Corn Syrup C 4%
wet 7.4 49.4 8.5 98.8 95.2 67.4 53.0 20.0 2.4 0.8 13th Corn Syrup C 2% 6.4 68.6 15.5 96.4 87.4 56.4 43.8 16.4 0.8 0.0 14th water 4% 6.7 62.2 5.0 95.0 86.0 60.8 43.8 8.8 0.4 0.2 15th LD 6% 6.6 48.8 9.0 88.4 74.8 53.6 48.4 38.0 26.0 19.8 16 2% 8.6 52.2 7.0 86.6 69.4 41.8 35.4 24.6 15.2 11.2 17th 10% 8.4 56.2 52.0 "l Abrasion index = standard designation and measurement of hardness. 56, n tiny size or the number of ι used sieves to an M. * ■) The numbers 14. 20, 35, 42. 60. 80 and 100 indicate the standard J
to obtain.

No matter what type of agglomerating agent, while 2 and 4% additional amounts are tolerable in this example was added that were obtained.

The product was a coarser sugar than if no All sieving behavior with the exception of the

Agglomerating agent was added, or if those of the control and water addition tests were only water to boil before agglomeration 5 ° within acceptable limits, giving the behavior. All of the corn syrup products exhibited one of liquid dextrose (batch 17) the least of high caking tendencies, while that was all acceptable and almost unacceptable
Products according to the invention, wherein hydrolysates as The above agglomerates of batches 1 to 7

Agglomerating agent was added or when then compressed into tablets using didn't clump together at all. In addition, all 55 performed a conventional tablet machine and printing like 6- and 8% corn syrup additions to one of the items listed in Table VI. The following values were large loss of yield and are therefore not used.

Table VI

approach Own
Tilt
for caking .chatten the
U.N
acceptable Agglomerates
Reasons for the
Unacceptability Average
thickness
cm Tablets
Through
cut
Weight kg / cnrVcm 1
2
3 normal
strong
strong X
X Caking
Caking 0.94!
0.905
0.927 2.0738
1.8400
1.9490 0.219
0.323
0.648

11th 1 951 460 U.N
acceptable Reasons for the
Unacceptability f 12th Tablets kg / cm ² / cm X bad yield I. Through
cut
Weight 0.283 continuation X Caking 2.1555 0.653 Properties of the agglomerates X Caking 2.1086 0.702 approach Tilt
for caking X bad yield Average
thickness
cm 2.1792 1.195 4th strong X bad yield 0.928 2.1456 0.829 5. strong 0.959 2.0645 0.322 6th strong 0.963 2.2021 0.431 7th strong 0.907 2.1261 0.556 8th strong 0.888 2.1993 0.451 9 ") normal X Caking 1.007 2.1224 0.636 10 ") normal X Caking 0.983 2.0106 0.668 11 ") a little bit stronger X Caking 0.988 2.0567 1.63 12 ") a little bit stronger X bad yield 0.982 1.9867 0.416 13th strong X bad yield 0.916 2.2842 0.472 14th strong 0.918 2.3184 15th strong 0.985 16 normal 1.005 17th normal 1.1001

") Mixtures 9 to 12 are the hydrolyzate agglomeration tablets, all others are conventional tablets. The mixtures have the same numbers designation as in table V.

The values in Table VI show that all agglomerates with corn syrup and liquid dextrose are unacceptable either because of their tendency to cake too high or because of their low yield (as a result of breakage or dust). Only those agglomerates which use hydrolysates as agglomerating agents formed acceptable tablets both in terms of strength (that is, high yield) and also their anti-lump properties. Also, noticeably less pressure was necessary in most of them Cases to press tablets according to the invention.

Example 3

For comparison purposes, three test agglomerates and tablets were made from a dextrose filter cake. The first two tests used the composition of the invention, the third test used a common corn syrup as an agglomerating agent. Agglomeration was carried out in a Hobart granulator with steam jacket. The preparation conditions were as follows:

Table VII

The sieving behavior of these tests was as follows: Table VIII

Sieve (mesh) I. Attempt no. 3 Analysis% throughput 89.8 2 98.0 35 20 77.6 94.4 92.0 28 63.4 87.0 81.8 35 53.4 75.8 73.6 42 • 43.4 66.6 64.2 4 ° 48 32.2 54.8 53.4 60 22.4 40.4 41.2 65 14.2 27.0 29.2 80 8.4 15.6 16.4 45 100 3.2 7.6 3.2 150 1.4 1.6 0.4 200 0.6

The agglomerates so formed in the above tests were then divided into 20 tablets for each agglomeral compressed under the same tableting conditions. The following properties were obtained.

Agglomeration Agglomeration Amount of Inclination to medium temperature Agglomerates Together attempt medium bake No. (Weight HY *) 40 ⁰ C percent up HY ") 40 ⁰ C Sugar base) none 1 Corn syrup 40 ⁰ C 3% none 2 solids 3% very 3 5% plastic

·) HY = hydrolyzate, prepared according to the procedure in Example I. Method A, and essentially according to the analysis of the I0-DE product of Table I.

Table IX Average of 20 tablets

Attempt no. 1

⁶⁰ thickness (cm) 0.872 0.838 0.938

Weight (g) 1.9095 1.8804 1;

Breakage (kg / cnrVcm

Thickness) j 1.196 | 1.688 j 0.431

An analysis of the above page clearly shows the superiority of the agglomerates and tablets according to the invention of the invention over conventional agglomerates under

r.s

Turning corn syrup and tablets made from it. For example, if dry hydrolyzate even in smaller amounts than corn syrup solids is used, the result is a stronger tablet, as the comparison fraction values show.

Example 4

Following the procedure of Method B in Example 1, a hydrolyzate was prepared which had essentially the same analytical properties as in Table II (i.e. DE = 20.7, etc.). 5% of this dry agglomerating agent is added to a dextrose filter cake containing 12% water including water of hydration. The mixture was mixed thoroughly and then placed in a Hobart mixer equipped with a stirrer and steam jacket. The mixture was then agglomerated at 4O ⁰ C. The material obtained, with a water content below 10% v / u, is an acceptable agglomerate with good anti-caking properties. When compressed into tablets, the fracture strength was acceptable.

Example 5

Four hydrolysates were prepared, the first three according to method A of example 1. The analytical Properties of these three first hydrolysates essentially correspond to those of 5, 15 and 25 D. E. Hydrolysates of Table I. The fourth hydrolyzate was prepared according to Method C of Example 1 and conformed essentially to Pattern C in Table IV. Each of these hydrolyzates was when dry at 2% by weight sugar solids with a centrifuge cake mixed crystallized dextrose with a water content of 13% including the water of hydration. After mixing thoroughly, the crystalline dextrose was placed in a Hobart mixer at one temperature agglomerated at 45 ° C. All the agglomerates formed had good sieving behavior, hardness and anti-caking properties. Comparatively, the 15-D.E. had hydrolyzate agglomerate the best properties, while the 5- and 25-D. E. hydrolyzate agglomerate, although acceptable, the inferior ones were. Tablets made from these agglomerates had similar ones Properties, with the 5- and 25-D.E. hydrolyzate tablets being the inferior ones in comparison with the other two types of tablets, but they were also acceptable.

50 Example 6

Schung was then transferred to troughs, agglomerated and with hot air at 110 ° C for 3 hours dried. The agglomerated product formed was screened through a Tyler No. ΙΟ screen (U.S. No. 12), and the product passed through, taken as a yield, was 52% (that is 1717 g).

Approach B

The same procedure was followed here as in approach A ίο with the modification that 3% water (98 g) has been used. The yield found was 66% (202 μg).

The properties of the agglomerates formed are given in the following table

Production of sucrose agglomerates

Two approaches of sucrose agglomerates were like is made as follows:

Approach A

3175.2 g of premium essentially dry white centrifuge sucrose (water content 0.36 x / x) was dry blended with 4 % hydrolyzate (of sucrose weight), that is 127 g of essentially dry hydrolyzate, with a DE of 10. Mixing was carried out for 10 minutes in a Patterson-Kelly mixer, whereafter water? was added with "stirring for 5 minutes in. the added -Vassermenge was 6% by weight of the overall samtmiscnung (which is approximately 200 g). This Mi -

Table X

Centrifugal sugar
agglomeration

% Water ...
Sieve analysis
% Throughput
(Type r sieves)

10

14th

20th

28

35.

42

48

60

Mass density,

kg / m ³

0.36

100

99.5

91.7

45.8

11.5

5.9

2.9

0.7

791

(6% water)
after
Agglomerate.
dry
and seven

0.25

9V

69.6

39.4

13.9

2.0

0.4

650

(3% water) after agglomeration.
Drying and sieving

0.18

100.0.

79.7

48.8

24.4

7.4

4.3

700

According to these values, both batches of agglomerated sucrose have a larger particle size than the sugar used before agglomeration. Formulation A has a larger particle size ^r al APPROACH B. Comparison of the mass densities confirms this conclusion. The agglomerates produced, which also have good sieving behavior (essentially all particles are between No. 10 and No. 42 sieve size), were also very acceptable for the manufacture of tablets or for the sanding of sugar confectionery, such as e.g. B. Drops.

Example 7

125 g of sucrose were dry mixed with 125 g of dextiose and 8 g of the hydrolyzate used in Example 6. The mixture was then mixed thoroughly at a slow speed for 5 minutes after the addition of 10 ml of water and then further mixed at the speed to be increased for a further 2 minutes. The product was agglomerated and dried with hot air for about an hour. The dried product was then screened through a No. 10 sieve and the percent throughput, which was considered to be the product yield, was 81.6%. The agglomerated product had the following properties:

2521

Table XI

sample

% Water

Average mass density, kg / m ³ ..

D.E. (Dextrose equi valentine)

Sieve analysis% by gang durcn üieb-

meshes

10

14th

20th

28

35

42

48

60

65

80

100

150

200

30 / SO mixture

before agglomeration

4.6 823 49.3

100.0 100.0 99.9 99.7 90.9 76.3 62.3 54.2 49.5 45.2 38.9 25.1 15.2

SO / fO mixture

after agglomeration

2.3 527 4U

100.0

99 7

91.8

67.5

31.0

18.4

10.5

5.1

2.0

0.6

0.3

0.1

0.0

16 sample 50/50 mix
before the
Agglomerate 50 $ n money
lu h dem
Agglomerate ⁵ Sieve analysis% Av
gang (mesh sizes)
10 100.0
99.8
99.2 100.0
99.6
96.2 14th 98.0
89.6
TZ ₁ Z
55.0 89.8
56.6
20.0 20th 44.2
36.4 10.8
5.6 28 32.0
28.6 2.6
1.2 35 21.4
18.6 0.6
n.4 l \ £ 48 ¹⁵ 60 65 80 100 150 200

The product had excellent bulk density, sieving performance and flowability and was easily in Tablets transferred. As in the previous example, the hydrolyzate acted as both a binder as well as the crystals agglomerating agent.

The agglomerated product had excellent bulk density, sieving behavior and flowability and was easily converted into tablets. The above values illustrate that the hydrolyzate has both Binder between the sucrose and dextrose as well as acting as an agglomerating agent door the crystals.

Example 8

11.3 kg sucrose was dry blended with 11.3 kg dextrose using a Hobart mixer with a stirrer. 0.91 kg of the hydrolyzate used as agglomerating agent in Examples 6 and 7 were then added to this mixture and the mixture was mixed for a further 10 minutes. Then, ¹ A kg of water was added with further mixing for 2 minutes. This mixture was then placed in a steam jacketed hot air rotary dryer at 132 ° C door for 15 minutes. The agglomerated product was then screened with a No. 10 mesh screen and the percent throughput, viewed as product yield, was 75%. The product thus formed had the following properties:

Table XII Example 9

Typical candies were made as follows: 97.00 percent by weight of a dextrose or sucrose product (containing a low D.E. starch hydrolyzate) selected from any of the acceptable Products of the previous examples were made with 1.88% citric acid, 0.12% artificial Orange flavor and 1.00% magnesium stearate mixed. The mixture then became one Piece of candy compressed in a conventional tablet machine. The tableted product had good strength, good breaking strength and taste like other pieces of candy.

Example 10

Lactose in an amount of 100 parts was agglomerated by mixing crystalline or powdery ones Lactose with 3 parts of a starch hydrolyzate of low D.E. in the range from 10 to 13 and 3 parts of water. The mixture was passed through a granulator and dried to form agglomerates of a particle size substantially larger than that of the starting lactose.

The agglomerated lactose is particularly useful in food formulations which have rapid dispersibility in liquid or require the formation of tablets.

sample 50/50 mix
before the
Agglomerate 50/50 mix
after
Agglomerate Vo water .4.4
861 3.7
652 [Average
Mass density, kg / m '..
DF

Claims (1)

Patent claims: I. Agglomerated sugar product for the manufacture of edible tablets, characterized by a crystalline sugar, if necessary an addition of citric acid. Magnesium Clearal and Cincm Artificial (ieschmnckstoff. I to IO (iewiclUspiozcnl of a Sliirkehydro- lysais as agglomerating agents. which has been produced by an enzyme and / or acid treatment of a starch source and has a dextrose equivalent of 5 to 25 and a descriptive wrapping π is of 2.0, the descriptive ratio being the sum of the percentages of sugars (0 with the degree of polymerization I to 6. divided by the dextrose equivalent means. 2 Agglomerated sugar product according to claim I, characterized in that the crystalline sugar is dextrose. Sucrose. Lactose or a Mixture of the same.