DE1951460A1 - Agglomerated sugar products - Google Patents

Description

GPC International Inc. International Plaza Bngle Wood Oliffs, Hew Jersey, USA

Agglomerated sugar productsο

Priority i US patent application

No. 767 520 of October 14, 1968,

The invention relates to the production of agglomerated Sugar products and their use "* In particular, the invention relates to the particular usability of starch hydro" lysates of low dextrose equivalents (hereinafter referred to as with D.E. called) as an agglomerating agent for crystalline sugar.

Crystalline sugars used in the food and drug industries are generally of two major types. The first type is sucrose from sugar cane or sugar beet.The second type is dextrose, which is generally obtained by hydrolysis of starch stOxi monosaocharide.Because sugar in crystalline form is required by the food and drug industry, the crystallization is the uxkrißallized raw sucrose or Dextrose evidently a necessary G-ewinnoKg & method · The leohnik has therefore vislf Uolieh gt # ordtn © Yerfahren for the crystallization raw. u-Löht eni rekelt * Binea of the most common diessr ver <.fahrtsn vöb <öht narin, siuen i ^ iissallieierten Hohauoker in I; "dsun £ ^ a bri? ^ * n _P demi the solution to an oversaturated

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Concentrate on condition and focus on the oversaturated solution to be sown with already formed sugar crystals <»By subsequent Cooling the solution will form new sugar crystals «Ie and grow» NaGh forming the crystals will be the remaining Mother liquor separated from the crystals »The crystals are then washed and dried to produce the finished product crystalline sugar to be obtained

For many reasons, require foods "and Arzneimittleindustrie that crystalline sugar is agglomerated" one of the many areas _s is required after which crystalline sugar, is the production of edible tablets © The term "edible! Tablets" is well understood in the art, and it is Examples of edible tablets used here in their usual meaning include candies i peppermint tablets, medicinal pills, placebos and the like ©

Agglomerated crystalline sugar is generally produced by first producing a crystalline sugar according to the method just described with the modification, that before! drying or, if dry sugar is present, after moistening, an agglomerating agent is added to the Sugar is added «The sugar is then added according to usual Process agglomerates, e.g. at elevated temperatures below Using a granulator, then dried and as an agglomerated Granulated sugar product sold or consumed ©

Previously it was mostly common as agglomerating either a liquid sugars (for _e Bo a sugar solution) of the agglomerated type or a syrup Zob "corn syrup au use · For example, crystalline for agglomerating dextrose © ine liquid solution either dextrose or corn syrup generally used as an agglomerating agent ©

The technical usefulness of an agglomerated sugar depends to a great extent on the degree of its resistance to caking) its permissibility of igglomerate strength, its low dust, but ooh. from his Ability when used to make tablets that can be used

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_o to form a strong easily compressible tablet desired density is generally believed that the size of the agglomerate particles plays an important Roll® for any agglomerated sugar to acceptable sizes of these desirable properties applies to achieve · For example, for many agglomerated sugars "if the diameter of the agglomerated particles is decreased, the losses increase with respect to the tablet fracture, dusting and the like corresponding to, and production decreases _e Perner, if in this and other types of agglomerated sugar, the diameter of the agglomerated particles decreases, 'take the weight and volume into a tablet, resulting in a loss of compressibility at constant fill volume. The problem of dusting, breaking and compressing can therefore generally be minimized for any system using a particular agglomerating agent to form edible tablets therefrom when the agglomerated particles therein are relatively large, usually larger than about 200 microns and preferably larger than about 400 microns Sugar particles are collected by the sieve with a mesh size of about 65 or more (mesh number below 65), then the agglomerated sugar has properties which are particularly desirable for tablets *

In the previous use, the usual agglomerating agents were acceptable levels of sieving behavior, agglomerate properties and properties of the edible tablets only with Difficulty and using large amounts of agglomerating agents and get water · Sometimes, so ζ · Β · when sucrose or mixtures of sucrose and dextrose agglomerate should be, the agglomeration failed either completely, ο · · the agglomerates were only in rare cases of accepted ^, "& £ quality and were generally not reproducible" In many cases, when dextrose has been agglomerated,

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was the agglomerated product formed hur of low Qualitätο Such results appear to be a real problem for the entire relevant industry _β

It is the aim of the invention to provide this industry with new agglomerable products of dextrose, sucrose and / or mixtures of dextrose and sucrose, which contain an agglomerating agent, and with and agglomerated sugars manufactured tablets, which are all acceptable and mostly also of improved quality, and which Products eliminate or significantly reduce the technical problems mentioned

Another object of the invention is a new crystalline To create sugar product in agglomerated form, which can be easily tabletted, and its crystals are exceptional strong and to use as a new binder are well suited for the production of agglomerated crystal sugar ο

These objects are achieved according to the invention in that the usual hitherto used agglomerating be replaced by an agglomerating agent, commonly referred to as a starch hydrolyzate of low DE may also be referred _e By using this hydrolyzate can add new types agglomerated sugar and edible tablets are formed ₀

The novel agglomerated sugar products of the present invention comprise * a crystalline "sugar and an agglomerating agent from a starch hydrolyzate low D.E.what combination in the presence of sufficient water and duroh subsequent drying an agglomerate forms »As a result of the presence of the Hydrolyzate, the crystalline sugar easily agglomerates with the use of conventional agglomerating experiences to form a crystalline sugar agglomerate of strong particles, which

has excellent sieving behavior and pourability, and which less breakage and dust during storage and transport shows as usual sugar agglomerates

Crystalline sugars useful in the invention include

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all types of crystalline sugar products, such as dextrose, Sucrose, iiaetose, and the like, and mixtures thereof · Many

these types of sugar are known in practice and are commercial items available under various trademarks · Such types of sugar are generally classified according to customary Process produced and crystallized

The crystalline sugar types which can be used according to the invention can be mixed with the agglomerating agent either in dry or in wet form crystalline sugars one which is in its centrifuge cake form after its crystallization, which Cake washed and centrifuged to a water content excluding the water of hydration, which, if present, is about 1 - 16 # of the cake weight Most of the time, the water present in this cake will be enough to generate the necessary amount of water to agglomerate the To provide sugar. This amount of water necessary for agglomeration of the mentioned product according to the invention excluding the water of hydration is generally about 1 to about 8 Grew <> # of the entire product

As already mentioned, the agglomerating agent used according to the invention can generally be defined as starch hydrolyzate of low D.E. <> These hydrolysates are used in an amount of from about 1 to about 10 weight percent of the sugar solids and preferably from about 2 to about 4 wt.

The low DE starch hydrolysates used in the present invention to produce crystalline sugar agglomerates are a relatively new class of starch material. These starch hydrolysates are prepared by subjecting a starch source to enzyme or acid treatment or a combination of both. It is important that the starch hydrolyzate have a relatively low DE · less than about 25 and preferably a DE · in the range 5-25 · The preferred materials have a DE within the range 10 to 15 · "» "" »* * ^g * Such starch hydrolysates have been found to be excellent agents for reducing the

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Reduce moisture uptake of normally hygroscopic foods while using other hydrolyzates from a D.E * significantly outside of this range to inferior products, which still have a show a tendency to absorb moisture and therefore tend to stick together or become sticky · ■

The term D.E »is used here to refer to G-e content of reducing sugars of the dissolved solids in one

Starch hydrolyzate expressed as a percentage of dextrose.

The starting starch, which is subjected to the hydrolysis treatment, can come from a wide variety of starch materials, such as ZoB ₀ cereal starches, waxy starches and / or root starches.Typical for these groups are maize, potato, tapioca, grain sorghum and wax milo -, waxy maize, rice starch and the like «The term" starch hydrolyzate "as used herein includes hydrolyzed starch materials from a wide" range of known starch sources "

As already mentioned, those are preferred for the invention Starch hydrolysates those with a D.Ee between about 5 to about 25, which can be produced by any desired process «

In a method designated in Example 1 under method A, a starch, Z ₀ B ₀ wax starch, is treated with a single egg-liLjIfVi.liebere'.4u η ^ bacterial alpha-amylase. In this process, an aqueous paste of waxy starch with a solids content of less than 50% is subjected to the hydrolysis action of bacterial alpha-amylase under suitable fermentation conditions to obtain a starch hydrolyzate. The hydrolyzate can also

characterized by having the sum of percent "rates (dry basis) of saccharides" having a degree of polymerization of 1-6 divided by the DE · to give a ratio greater than about 2.0 · this ratio becomes referred to as the characteristic or descriptive relationship. These low DE * products with a descriptive ratio of less than about 2 are about ⁵ undesirable because they have, for example, less water solubility and

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also tend to "form opacities in solution" in comparison to products with a ratio of at least 2 «

The same product as described above can also be produced in other ways »For example, a mixture made from starch and water with less than $ 50 solids first subjected to the hydrolysis action of a bacterial alpha-amylase and then subjected to a high temperature heating step to make any undissolved starch soluble.Because this temperature tends to inactivate the enzyme, it is then necessary to hydrolyze the solubilized partial to cool and to subject to a second hydrolysis by treatment with additional bacterial alpha-amylase to obtain the sole starch hydrolyzate · This procedure is referred to in example 1 as method B »

A third method of making the preferred class of low D.Ee starch hydrolysates, as Method 0 im Example 1, is to hydrolyze a mixture of starch and water by the action of acid in order to to achieve a D.Ee between about 5 and about 15 · The partial hydrolyzate is then subjected to the action of bacterial alpha-amylase to produce a starch hydrolyzate with a D.E. from about 10 to about 25 to win

A starch hydrolyzate which is particularly preferred for the invention has the following characteristics: Water content approximately at most and a D.E * from 10 - 13 *

As already indicated, the agglomerated products are preferably formed by adding a dry, low DB starch hydrolyzate agglomerating agent to the wet crystallized sugar DE are brought into solution first, welohe up to about 60 i »solids with sufficient water has to. 1 - 16 wt # of water in the finished agglomerated products provide · This solution can advertising added then dry granulated sugar with mixing or spraying

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Instead, the agglomerated product according to the invention can be formed in situ by letting water, drier Granulated sugar and the dry agglomerating agent with so ge. low moisture like $ 2 are mixed together »

Regardless of the method by which they were obtained, the agglomerierbaren products of the invention are easily agglomerated using conventional methods The agglomerated product thus formed have excellent screening behavior, not cake, have flow and contain strong agglomerated particles which do not dust and not getting broken ₀ Furthermore, the agglomerated products have high water density and compressibility and can therefore easily be processed into strong, edible tablets using conventional methods.

In a typical example of the invention and its application, an agglomerated product has been formed by 97 Parts by weight of wet dextrose crystals and 3 parts by weight of a starch hydrolyzate of 10 D.E. were mixed, the The water content of the mixture is between 2-4% by weight only

of the water of hydration. The mixture was then passed through an agglomerator (e.g. an Oolton granulator) and dried · The crystalline agglomerates came out of the dryer with the usual water contents · The agglomerates proved to be of a hard crystalline nature © Wenn subjected to pressure, e.g. in a conventional tablet machine, require the agglomerates only about half of the usual pressure, as is generally used to form a strong tablet is required

Articles made in accordance with the present invention include all types and shapes of pressed or extruded agglomerated ones Sugar products. The basic breakdown of these articles comprises an agglomerated sugar and a low D.E. starch hydrolyzate. In the case of placebos it is generally no further additives in the tablet or pill in the case of sugar confectionery, such as candies, peppermills, candy cigarettes, and the like can be conventional flavorings

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such as citric acid, Eetsyn, chlorophyll and the like are added will. Purely medicinal pills will be the "concerned" Medicine, vaccine, antibiotics and the like added in the usual dose »

The agglomerable compositions and agglomerates according to the invention find many applications in food and pharmaceutical industry. Apart from their usefulness in the manufacture of edible tablets already mentioned they are used in other areas, e.g. those where rapid dispersibility in water, uniform coarse particle size, Security against breakage and dust and the like is desired *

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

example 1

The following specific procedures illustrate those already mentioned three basic processes for making starch hydrolyzates of low D.E., which are used as agglomerating agents according to the invention

Mejbhode ^ A - einufijgejä enzyme process

An aqueous starch slurry was prepared with a content of 30 wt. # Solids from Wachsmilostärke "The temperature of the slurry was raised and maintained 85-92 ⁰ O. A bacterial alpha-amylase preparation was added in an amount just above 0.025 wt. # Of thickness within a time of a little more than 30 minutes · The mixture was d _a ^ n held at the same temperature for a further 30 minutes · The temperature was then lowered to less than 80 ⁰ O, 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 ⁰ O in order to inactivate the enzyme and terminate the conversion.

The following table I shows typical saccharide analyzes of low hydrolysates obtained according to this process

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D, E. DP denotes the degree of polymerisation * DP ₁ represents the total amount, expressed in percent by weight dry basis, of monosaccharides present in the hydrolyzate «DPg indicates the total amount of disaccharides present in the hydrolyzate, etc.«

Table I.

Typical saccharide analyzes

DoB,

10 15 20 25

Hydrolyzate
composition 0o1 0.3 0.7 1.4 2.4 DP ₁ 1.3 3.4 5.5 7.6 9 * 7 DP ₂ 1.8 4.3 6-9 9.4 12.0 DP ₅ 1.8 3.5 5.2 6.9 8.6 ^DP 4 1.8 3.6 5.5 7 * 4 9.3 DP ₅ 3.3 7.0 10.6 14.3 18.0 ^DP 6 89o9 77.9 65.6 53.0 40.0 DP ₁ , and higher 10.1 22.1 34.4 47.0 60.0 Total DP ₁ y ₇ 6 Descriptive ratio 2 _e 0 2.2 2.3 2.4 2.4 Method B - two-step enzyme-enzyme process

Unmodified corn starch was suspended in water to give an aqueous suspension containing 28-32% by weight of the unmodified corn starch. The pH was adjusted to 7.5-8.0. ΗΪ-1000 bacterial alpha-amylase (manufactured and sold by Miles Chemical Laboratories) to this mixture in an amount of 0.05 based on the starch solids added 'This starch suspension was added over a period of 30 minutes to a to a temperature of 90 - 92 ⁰ O held container added with stirring. After completion of the Siärkezusatzes the liquefaction was continued for 60 minutes, after which time the hydrolysis was within a DE region of 2-5 · The liquefied starch was then heated to 15O ⁰ O and

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The heat treatment was held at this temperature for 8 minutes destroyed the remaining enzyme activity and led to reduced yield losses in the filtration ©

Further saccharification to the eventual DoB. was "caused by the addition of more HT-1000 bacterial alpha-amylase after cooling the liquefied starch hydrolyzate to a temperature suitable for conversion. The liquefied starch was ^{cooled to 80-85 0} O and HT-1000 in an amount of 0.02 Gewe # of starch solids added · After 14-20 hours of conversion time, the desired final D.Jäe was obtained (2O) ₀

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

Table II

Dole DP ₁ DP ₀ DP ,, DP. DP _K DP ^ DP ₇ ^ Descriptives __L_ _L _JL -JL -JL JL - ratio

20.7 2.4- 7.5 10.8 8.0 6.8 15.1 4-9 * 4 2.4

Method ^ Q - two £ tufi ^ ges__Säu £ e-enzyme methods

Different samples of corn starch (A, B and G) were clipped in water to obtain porridges with Baume ranges from 14 ° to 22 °. These pulps were partially acid hydrolyzed to a maximum of 15 DoE. The particular DE achieved by acid hydrolysis for each of the samples is given in Table III. After the acid hydrolysis, the slurry was neutralized to a pH between 6 and 7. The neutralized liquid was cooled to 80-85 ⁰ O and treated with bacterial alpha-amylase (HT-1000) in an amount as indicated below. A final DE of 19 -21 was obtained for each of the mothers in a time between 1 and 3 hours. The final conversion fluids are faint in color. These liquids are lightly refined and evaporated to about 42 ° Bäume to make syrups. Dry products can be obtained - too. Tables III and IV give the reaction conditions for the conversion and the product analysis

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sen again »

Table III

195Η6Ό

DE des
Acid hy-
drolysats Enzyme Conversion Conditions PH Enzyme-
dose Time
Hours. end
DE template 15.2
12.9
10o3 $> Dry temp.
substance o «
\ j 6.5
6.5
6.5 0.01
0.05
Oo 1 1
2
2 19.7
20.2
21.8 A.
B.
C. 38 80
37o5 85
38o1 85 Table IT Product analysis

Sample end- $> dry- DP1 DP DE kensubstanz

DP, DP

DP

(■ DP ₇ , Descripti ^b ' ⁺ ves ratio

A 19o7 B 20.2 0 21.8

72 72 75

3.9 5.8 8.2 7o2 7.3 10.2 57.4 2.1 2.3 5.9 8.5 6.4 6.6 12.6 57.7 2.1 2o3 8.3 10.9 8.1 9.2 16.9 44.3 2.5

Example 2

Production of crystalline dextrose agglomerates

A starch hydrolyzate having a DE of approximately 10 was prepared by following the procedure of Example 1, Method A. The analysis of this product was essentially the same as the analysis of the 10 DE product in Table I. Two batches of centrifuge cake sugar crystalline dextrose, from each weighing 22.7 kg were mixed with the hydrolyzate, the hydrolyzate being added in an amount of 2 and 4 wt. # solids and used either dry or with a small amount of water as indicated in Table V · The original centrifuge cake before Hydrolysatzusatz contained about 12 to 15 96 water wherein about 9 i "hydration water is included. After mixing the dextrose with the low DE hydrolyzate for about

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10 minutes in a conventional mixing machine, the mixture was transferred to a hot-air rotary dryer with a steam jacket at a temperature of 132 ⁰ O. After a drying time of 15 minutes, the dry product was _{sifted using a Tyler No. 8} 10 sieve and the percentage throughput as yield (dohe as Product) viewed · The agglomerated products had the sieving behavior given in Table V »

For comparison purposes, the same basic procedure as described was carried out again with the modification that instead of using the hydrolyzate of low D.Bo conventional and comparable amounts of common agglomerating agents were used, namely liquid dextrose and corn syrup ( $ 60> solids) _o three different Types of common corn syrup were used · In addition, an experiment was carried out with complete omission of an agglomerating agent · This experiment is considered a control and is labeled Run 1. Another experiment was carried out with the addition of only $ 2 of water to the cake

without the addition of any agglomerating agent (batch 16). For comparison purposes, Table V includes the sieving behavior and other properties of these common agglomerates. "

For the sake of simplicity, the hydrolyzate is labeled HY and the liquid dextrose ID in the table

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Sowing «additional amount no - water A. I. , 42, 60 , 80 Tabel T Cb) the 20th 4th 35 4th 42 6th 1 » throughput 80 100 t Corn syrup A 2 - 6 "Number of sieves used, " 8th 4th 60 1 Corn Syrup A $ 4 8.9 82o4 Ca) # _about r- 14th , 6 98o 90, 4th 860 8th 38o4 I80O I. 2 Corn Syrup A $ 6 80I 6808 size 06 98 0 860 0 77o 4th 73.8 I606 1.2 3 Corn Syrup B $ 2 7.6 4608 4o0. 99 o2 9I0 62, 4th 47 0 6th 39o2 Ό.8 0o4 4th . Painting syrup B 4 # 9.4 11.4 5.0 99 06 38 0 3o 2 1o 4th 12o6 OoO OoO ■ 5 Corn syrup B 696 8.4 39o4 IO0O 97 oO 96o 74o 0 62o 8th 0o4 3o6 O08 6th Corn syrup B 89ε 808 38o0 24o5 71 06 860 49o 4th 33. 6th 25o8 2o4 1.0 7th Ηϊ 2j6 dry 8o5 28oO 4o5 99 oO 6Oo 2Oo 4th 11. 4th 11.4 1.2 0.4 _i O
O 8th Ηϊ 4? Ί dry 5.9 ' 37o2 13o0 96 o2 6Oo 26o 8th I80 0 4oO 1.4 O08 to (D
OO 9 Ηϊ 2 ^ NaJB 806 46o2 4O0O 91 08 95o 7I0 2 6Oo 0 6o4 7o8 2o6 cn to 10 Ηϊ 4 # wet 7.1 60.8 69.0 82 0 4 93o 7I0 2 59o 2 32o8 5oO 2oO ίί 11th Corn syrup C $ 2 8o3 44o0 7o5 98 oO 95o 66o 4th 57o 0 26oO 8o2 3o2 CO
CD 12th Corn syrup C $ 4 7.4 49o4 13o0 97 "8th 860 54o 4th 42o 8th 3O06 5o6 2o4 σ » 13th Corn syrup C 69ε 6o4 6806 8o5 99 08 95o 67 « 8th 53c 8th 20o2 2o4 O08 14th Waeser $ 2 6.7 62o2 15.5 96 o4 87o 56o 6th 43o 4th 2O0O O08 OoO 15th U) 103ί 606 4808 5o0 98 oO 860 60, > 8 43c 4th 16.4 0o4 0o2 16 ₁ 806 52o2 9.0 96 o4 53c 48 0 808 26.0 19.8 17th 8o4 56o2 7o0 95 06 41 « 35c 38o0 15o2 11.2 52.0 88 24o6 (a) Abrasion index β standard designation 56oQ 86 and measurement of the 0>) Numbers 14., 20, 35 and give 100 Standard mesh size or the to a measure too Sieving behavior 5 received0 8th 2 4th 2 8th 4th 0 4th 6th 6th 2 6th 2 4th Q 74o8 69. hardness

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Regardless of what type of agglomerating agent was added in this example, the product obtained was a coarser sugar than if no agglomerating agent was added or if only water was added to the cake before agglomeration _c All corn syrup products showed a high tendency to cake, while the products according to the invention, where hydrolysates were used as agglomerating agents, clumped together little or not at all. In addition, all six and eight percent corn syrup additions led to too great a loss of yield and could therefore not be used * while 2 and 4 additional quantities were tolerable · All sieving behaviors with the exception of those of the control and water addition trials were within acceptable limits, with the behavior of liquid dextrose (batch 17) being least of all acceptable and almost unacceptable

The above agglomerates of Forms 1-7 were then compressed into tablets using a conventional tablet machine and printing as shown in Table VI. The following values were obtained

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Table YI VA affiliations of the Asslomerate Caking acceptable X Tablets o, 941 2.0738 0.219 f Approach Neisiune to the inappropriateness normal X 0.905 1.8400 0.323 strong X 0.927 1.9490 0.648 Ch 1 strong X Reasons for the average- average- kg / cm / cm 0.928 2.1555 0.283 2 strong X Unacceptability
cm weight 0.959 2.1086 0.653 3 strong X 0.963 2.1792 0.702 4th strong X Caking 0.907 2.1456 1.195 O
ί— » 5 strong Caking 0.888 2.0645 0.829 (O 6th strong bad yield 1.007 2.2021 0.322 00
NJ 7th ⁸ V 'normal Caking 0.983 2.1261 0.431 O 8th ^a 'normal Caking 0.988 2.1993 0.556 _ ^ - » 9 ( ^& 'a little stronger X bad yield 0.982 2.1224 0.451 CD
cn 10 ( ^a 'somewhat stronger X bad yield 0.916 2.0106 0.636 CD 11 ^ strong X 0.918 2.0567 0.668 O 12 ⁽ strong X 0.985 1.9867 1.63 13th strong X 1.005 2.2842 0.416 14th normal 1.1001 2.3184 0.472 15th normal Caking Approaches 9-12 are the hydrolyzate agglomerate tablets, all others are common 16 Caking Tablets The batches have the same lobster designation as in Table Yo 17th Caking (a) bad yield bad yield

The values in Table VI show that all agglomerates with corn syrup and liquid dextrose were unacceptable, either because of their high tendency to cake or their low yield (as a result of breakage, dusting and the like]) Only those agglomerates, which hydrolyzates agglomerate, ttel used formed acceptable tablets in both respects the strength (doi * high yield) and also its anti-lump properties, In addition, noticeably less pressure was necessary in most cases in order to produce tablets according to the invention to press.

Example 3

For comparison purposes, three test agglomerates and tablets were used produced from a dextrose filter cake The first two tests used the composition according to the invention, the third test used a common corn syrup as an agglomerating agent. Agglomeration was carried out in a Hobart steam jacketed granulator. The approach conditions were the following »

attempt
No.

Agglomerates
middle

Table VII

Agglomeration temperature

Amount of agglomerating agent (Grew. $ Based on sugar)

tendency to cake

HY
HY

40 ⁰ O 40 ⁰ O

3 corn syrup solids

4O ⁰ O

none none very plastic

(a) HY - hydrolyzate prepared according to the procedure in Example 1, Method A and essentially according to the analysis of the 10 DB product - of Table I ₀

The sieving behavior of these tests was the following «

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Table VIII

attempt
Sieve (mesh)
Analysis jo throughput

35

42

48

80 100 150 200

The agglomerates formed in the above tests were then converted into 20 tablets for each agglomerate under the same tableting conditions Compressed to The following properties were obtained

Table IX

89.8 94.4 98.0 77.6 87.0 92.0 63.4 75.8. 81.8 53.4 66.6 73.6 43.4 54.8 64.2 32.2 40.4 53.4 22.4 27.0 41.2 14.2 15.6 29.2 8.4 7.6 16.4 3.2 1.6 3.2 1.4 0.6 0.4

Attempt ITr ₀ average from 20 Tablets 1 2 3 Thickness (cm) 0.872 0.838 0.938 Weight (g) 1.9095 1.8804 1.8808 Breakage (kg / cm / cm thickness) 1,196 1.688 0.431

An analysis of the above values clearly shows the superiority of the agglomerates and tablets according to the invention usual agglomerates using corn syrup and tablets made from it »If, for example, dry hydrolyzate even in lesser amounts than corn syrup solids is used, the result is a stronger tablet like the one Show comparative gross values "

Example 4

Following the procedure of method B in example 1

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A hydrolyzate was produced which had essentially the same analytical properties as in Table II (doie D.Eo = 20.7 USWo). 5% of this dry agglomerating agent are added to a dextrose filter cake containing about 12% water including water of hydration the mixture was thoroughly mixed and then placed in a Hobart mixer, who was equipped with a stirrer and a steam jacket ₀ the mixture was then stirred at 40 ⁰ O the material obtained agglomerated with a water content below 10 $ was an acceptable agglomerate with good * Antiklumpνermögen ο If Compressed into tablets, the result was an acceptable breaking strength

Example 5

Four hydrolysates were prepared, the first three according to method A of Example 1 _e. The analytical properties of these three first hydrolysates essentially correspond to those of 5 DoEc, 15 D.Ee and 25 D.Eo hydrolysates in Table I ₀ the method of example 1 and was substantially the same pattern C in Table IV ₀ Each of these hydrolysates is in a dry state in an amount of 2 Gewo # sugar solids thoroughly with a centrifuge cake of crystallized dextrose having a water content of about 13 $, including the hydration water mixed After crystalline dextrose was mixing in a Hobart mixer at a temperature of 45 ⁰ C, agglomerated any agglomerates formed besaßon good sieving, hardness and Antiklumpvermögeno Comparatively possessed the 15 DE ₆ hydrolyzate agglomerate the best properties, while the 5 DE and 25 DE " Hydrolyzate agglomerate, although acceptable, the minor w tablets made from these agglomerates had similar properties, with the 5 D.Eo and 25 DE hydrolyzate tablets being the lower quality ones compared to the two other types of tablets, but they were also acceptable.

Example 6

from

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Two batches of sucrose agglomerates were made as follows:

Approach Ai

320 g of premium essentially dry white centrifuge sucrose (Water content $ 0.36) were dry with $ 4 hydrolyzate (of sucrose weight) doio 127 g of an essentially dry hydrolyzate with a D.E ο of about 10 mixed o Mixing was carried out for 10 minutes in a Patterson-Kelly mixer, followed by water slowly was added with stirring for 5 minutes ο the added Amount of water was $ 6 the weight of the total mixture (doie approximately 200 g) o This mixture was then poured into troughs transferred, agglomerated and with hot air of 110 ° 0 during

Dried for 3 hours. The agglomerated product formed was _{screened through a Tyler No. 0} 10 sieve (TJeS-. Ho. 12) and the product passed through, considered as a yield, was 62 # (i.e. 1717 g) «

Approach Bt

The same procedure was followed here as in batch A with the modification that 3 $ water (about 98 g) was used ". The found yield was $ 66 (about 2023 g) β

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

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Table X

Centrifugal- A (656 water) B {% water) sugar before after agglomeration- after agglomeration, lomerization, drying and drying and sieving

agglomeration

i> water

Sieve analysis
$> Throughput

Tyler
Sieves

10 H 20 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

0.25

93.7

69.6

39.4

13.9

2.0

0.4

0.18

100.0

79.7

48.8

24.4

7.4

4.3

650

700

According to this fourth both approaches have from agglomerated sucrose a larger particle size than that used twitches r prior to agglomeration · batch A has a larger particle size than approach B. Comparison of the mass densities confirms this conclusion _β The agglomerates produced which exhibit also good sieving, (in substantially all of the particles are between Hr. 10 and No. 42 mesh size _β), were also very acceptable for the preparation of tablets or for the sanding of confectionery, such as ζ · · β Drops _β

Example 7

125 g of sucrose were dry mixed with 125 g of dextrose and 8 g of the hydrolyzate used in Example 6. The mixture was then mixed thoroughly at a slow rate after the addition of 10 ml of water and then further mixed at an increasing rate for a further 2 minutes agglomerated and dried with hot air for about an hour . The dried product was then duroli tin Ir. 10 sieve sighted, and the percentage through *

♦ 5 minutes

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rate, which was taken as the product yield, was 81. The agglomerated product had the following properties:

! Table XI

Template" 50/50 mix before Sieve analysis # passage
through sieve mesh 100.0 50/50 mixture according to agglomeration 10 100.0 agglomeration $ Water 4.6 H 99.9 2.3 Average
Mass density kg / m3 823 20th 99.7 527 DoEo (dextrose
equivalent to) 49.3 28 90.9 41.3 35 76.3 42 62.3 100.0 48 54.2 99.7 60 49.5 91.8 65 45.2 67.5 80 38.9 31.0 100 25.1 18.4 150 15.2 10.5 200 5.1 2.0 0.6 0.3 0.1 0.0

The agglomerated product besaßX ffließvermö'gen excellent bulk density, and sieving properties and was easily converted into labletten · explain the above values that the hydrolyzate and also acts both as a binder between the sucrose and dextrose as an agglomerating agent for the crystals XtXHX ·

Example 8

11.3 kg sucrose were dry with 11.3 kg dextrose under Using a Hobart scissors mixed with a stirrer 0.91 kg of that in the examples were then added to this mixture 6 and 7 old aeglomerism agents used hydrolysates

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"Ben and the mixture mixed for a further 10 minutes _o Then about 1/2 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 for about 15 minutes ") The agglomerated Product was then _{screened with a No. 0} 10 mesh screen and the percent throughput, viewed as product yield, was 75 ° The product thus formed had the following properties:

Table XII Sieve analysis 56 pass
(Machine sizes) 100.0 50/50 mixture according to
agglomeration Pattern 50/50 mix before
agglomeration 10 99.8 3.7 io water 4.4 H 99.2 652 Average ^
Mass density ig / m 861 20th 98.0 DoEo ■ art 28 89.6 35 72.2 100.0 42 55.0 99.6 48 44.2 96.2 60 36.4 89.8 65 32.0 56.6 80 28.6 35.8 100 21.4 20.0 150 18.6 10.8 200 5.6 Owned the product 2.6 1.2 0.6 0.4 aete mass density. she

behave and flowability and was easily made into tablets Converted · As in the previous example, the hydrolyzate acted as both a binder and the crystals agglomerating agent

009820/1764

Example 9

Typical candies were made as follows:

About 97,100 wt * $ of a dextrose or suerose product (containing a low D ₀ E ₀ starch hydrolyzate) selected from one of the acceptable products of the previous examples was added with $ 1.88> citric acid, $ 0.12 artificial orange flavor and $ 1.00 magnesium stearate mixed to The mixture was then compressed into a candy bar in a conventional tablet machine * The tableted product had good strength, good breaking strength and a taste like other candy bars *

Example 10

Lactose in an amount of 100 parts was agglomerated by mixing crystalline or powdered lactose with 3 parts of a starch hydrolyzate of low DoEo im Range of 10-13 and 3 parts of water o The mixture was made sent through a granulator and dried to form agglomerates of a particle size in the 3ESSKS substantially larger than that of the starting lactose *

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

00982 $ 0/17

Claims (1)

7 · Claims 1 ο agglomerated 1ree sugar product labeled through a crystalline sugar and an agglomerating agent, which is a starch hydrolyzate with a DoBo of about 5 "to about 25, which combination in the presence of sufficient water and after subsequent drying an agglomerate forms « 2 · Agglomerated sugar product according to claim 1, characterized in that the crystalline Ordered sugar made from dextrose, sucrose, lactose or mixtures thereof 5β agglomerated sugar product according to claim 1 or 2, characterized in that the starch hydrolyzate has a D.Eο of about 10 to about 15 » 4o agglomerated sugar product according to the preceding claims , characterized in that the starch hydrolyzate has a water content below about 5 $ and a D.E. from about 10 to about 13 5. Agglomerated sugar product according to the preceding claims , characterized in that the starch hydrolyzate in an amount of about 1 to about 10 Gew »# is present * 6ο Agglomerated sugar product according to the preceding claims , daduroh characterized in that the starch hydrolyzate in an amount of about 2 to about 4 Grewe? I present isto 7ο Agglomerated sugar product according to the preceding claims » _daduron characterized in that the starch hydrolyzate has a deacriptive ratio of about 2.0, the descriptive ratio being the sum of the percentages of saccharides with the degree of polymerization (J O 9 8 2 O / 1 7 6 4 ORIGINAL INSPECTSD I meant to 6 divided by the DoEo 8β Agglomerated sugar crystals characterized by a larger proportion of sugar and from about 1 to about 10 wt. Of a starch hydrolyzate of low DoEo with a DoE ₀ of about 5 to about 25 o 9β agglomerated sugar product according to claim 8, d a through indicated that the sugar is dextrose, sucrose, lactose or a mixture thereof « 10o agglomerated sugar product according to claim 8 or 9 »characterized in that the starch hydrolyzate of low DoEo in an amount of about 2 until about 4 Gewo $ is present « II ο agglomerated sugar product according to claim 8, 9 or 10, characterized in that the strength " hydrolyzate a DoE. owned by about 10 to about 15 12o edible tablet characterized by an agglomerated crystalline sugar and a starch hydrolyzate from a low DoEo with a D.Eο from about 5 to about 25β 13o edible tablet according to claim 12, characterized by a further content of citric acid, Magnesium stearate and an artificial flavor « 14. Edible tablet according to claim 12 or 13, thereby characterized in that the agglomerated crystal Sugar consists of dextrose, sucrose, lactose or mixtures thereof o 15. Edible tablet according to claims 12, 13 or 14, thereby g θ k β 'η η indicates that the starch hydrolyzate has a D.Eo of about 10 to about 15 16a edible tablet according to claims 12 to 15, d a du raw marked that the starch hy- U09820 / 1764 drolysat a water content under about $ 5 and a DoEe of 10-13 owns 17o edible tablet according to claims 12 to 16, characterized in that the starch hydrolyzate in an amount of from about 2 to about 4% by weight of the sugar present isto 18o edible tablet according to claims 12 to 17, characterized in that the starch hydrolyzate has a descriptive ratio of at least about 2, where the descriptive ratio is the sum of the percentages of saccharides with a degree of polymerisation from 1 to 6 divided by the DoEo means 19. A method for agglomerating a crystalline sugar, characterized in that a starch hydrolyzate of low DoE ₀ , which has a DE of about 5 to about 25, is added to this sugar before agglomeration 2Oo method according to claim 19 ι characterized in that that the crystalline sugar consists of dextrose, sucrose, lactose or mixtures thereof. 21c The method according to claim 19 or 20, characterized in that the starch hydrolyzate has a DoEo of about 10 to about 15 ₀ 22o method according to claim 19 to 21, characterized that the starch hydrolyzate is added in an amount of about 1 to about 10 wt% of the sugar willo 009820/1764