By fluidized-bed spray granulation, dextrin granules having a high content of enclosed alcohol are obtained from dextrin/water/alcohol mixtures.

BACKGROUND OF THE INVENTION 
1. Field of the Invention 
The present invention relates to granules having a relatively high content 
of ethanol (below "alcohol") and a process for the preparation of 
alcohol-containing granules by fluidized-bed spray granulation. 
2. Discussion of the Background 
It is known that alcohol-containing instant beverage mixtures may be 
produced by adsorption of alcohol-containing components to non-volatile 
components (German Offenlegungsschrift 195 00 919). Fixing the alcohol to 
the surface by adsorption cannot ensure permanent encapsulation of the 
alcohol, which greatly restricts the handleability and leads to high 
alcohol losses in the unpackaged state. In particular, these powders are 
not free-flowing. 
It is further known that alcohol-containing powders having a high alcohol 
content and high alcohol yield can be produced (German Patent 
Specification-C 32 14 321; U.S. Pat. No. 4,454,165) by spray-drying 
hydrolyzed starch containing at least 50% oligosaccharides having a degree 
of polymerization of glucose of up to 8 and containing up to 10% 
saccharides having a degree of polymerization of glucose of up to 2 in an 
alcohol-containing aqueous solution. The requirements made of the support 
in this process with respect to the degree of polymerization restrict the 
usable materials greatly, however. Moreover, the particle properties 
(size, structure) can only be varied in a limited manner. 
SUMMARY OF THE INVENTION 
The object of the invention was therefore to provide alcohol-containing 
granules which do not have the disadvantages described. 
We have now found a process for the preparation of alcohol-containing 
granules by encapsulation using dextrins, which is substantially 
independent of the degree of polymerization of glucose of the dextrins 
used. Depending on requirements, porous or compact granules can be 
produced having a high alcohol content, with effective alcohol 
encapsulation and good flowability. 
The process according to the invention is therefore not directed to a 
particular content of G.sub.3 -G.sub.6 oligosaccharides (G represents 
glucose, the indices the degree of polymerization). 
The invention relates to a process for the preparation of 
alcohol-containing granules by fluidized-bed spray granulation of a 
solution of dextrins in a water/alcohol mixture.

DESCRIPTION OF THE INVENTION 
The term "solution" for the purposes of the invention also includes 
dispersions. Preferably, however, true solutions (which therefore do not 
include dispersions) are used. 
The process according to the invention permits the use of saccharides which 
have virtually no alcohol-covering properties and can only be processed to 
give powders with difficulty using conventional methods. By this process, 
surprisingly, very high yields of encapsulated alcohol, based on the 
alcohol used, may be achieved. 
The term "dextrins" is taken to mean starch, waxy starch, modified starch, 
modified waxy starch, preferably starch breakdown products, in particular 
cold-water-soluble starch breakdown products. "Modified starch" is taken 
to mean starches and starch breakdown products which are altered by 
chemical derivatization, principally esterification or etherification. 
"Starch breakdown products" for the purposes of the invention primarily 
include products obtainable by acid-catalyzed hydrolytic breakdown or by 
enzymatic breakdown; the enzymatic breakdown, as is known, can be 
performed with the use, for example, of amylases, glucoamylases or 
pullulanases. Preferred dextrins include starch breakdown products having 
a content of G.sub.1 -G.sub.2 saccharides of greater than 10% by weight 
and of G.sub.1 -G.sub.8 saccharides of less than 50% by weight. 
Particularly preferred dextrins are pregelatinized (cold-water-soluble) 
starches. 
In particular, preference is given to dextrins which are soluble at a 
concentration of at least 40, preferably at least 50, in particular at 
least 60, % by weight in water at 25.degree. C. 
Mixtures of the dextrins described and cellulose or cellulose derivatives 
can also be used. Preferred mixtures comprise 50 to 99% by weight of 
hydrolyzed starch containing more than 10% by weight of saccharides of a 
degree of polymerization of glucose of up to 2, and 1 to 50% by weight of 
simple or modified starch, polysaccharides, cellulose, cellulose 
derivatives and/or gelatin. 
The solutions to be used for the process according to the invention 
generally comprise 20 to 70, preferably 35 to 55,% by weight of dextrins, 
10 to 40, preferably 20 to 35, % by weight of water, 10 to 40, preferably 
20 to 35, % by weight of alcohol and, if appropriate 20% by weight of 
other components, such as wine dry matter. The term "solution" for the 
purposes of the invention also includes non-true solutions and 
dispersions. 
The viscosity of the solutions to be used for the process according to the 
invention depends on the necessity of the mechanical atomization provided 
for the process; it is generally 100 to 200, preferably 140 to 170, 
mPa.s/30.degree. C. and a shear rate of 981 l/min. 
The solutions are spray-granulated in a fluidized bed with constant 
agitation. In the course of the fluidized-bed spray granulation, particles 
situated in a fluidized bed which are substantially smaller than the 
granules to be produced are sprayed with an atomizable starting material 
and dried until the particles have reached the desired particle size. 
A suitable process for the fluidized-bed spray granulation and a device for 
this process are disclosed, for example, by EP-A 163 836; U.S. Pat. No. 
(4,946,654) device of this type essentially consists of a fluidized-bed 
granulator 
which contains apparatuses for spraying the product fed in a sprayable 
form, 
which, in addition, contains a system suitable for recycling fine fractions 
escaping from the fluidized bed and 
to the gas-distributor plate of which, one or more counter-current gravity 
classifiers are directly attached. 
Granules having a narrow particle size distribution may be produced by 
a) spraying the product to be granulated in liquid form into a fluidized 
bed, 
b) separating off the fine fractions escaping from the fluidized bed 
together with the exhaust gas and recycling them to the fluidized bed as 
seeds for granule formation, 
c) solely by setting the classifying gas flow rate, influencing the 
granulation process in the fluidized bed in such a manner that granules 
are formed in the size preset by the classifying gas flow rate, and 
d) taking off the finished granules alone via one or more counter-current 
gravity classifiers inserted into the gas-distributor plate of the 
fluidized-bed apparatus and 
e) if appropriate, subjecting the granules thus obtained to a thermal 
aftertreatment. 
Advantageously, the process can be carried out in such a manner that the 
granule formation process, in the interplay between granule growth and 
seed formation, is inherently set to the discharged granule size 
predetermined by the classifying gas feed. In this case, the size of the 
granules can be set via the classifying discharge. These embodiments of 
the process are, for example, described in European Patent Specification 
332 031 (U.S. Pat. No. 4,931,174) and 332 929 (U.S. Pat. No. 5,213,820). 
In principle, the process can also be carried out using standard 
granulators continuously or batchwise. 
The classification can equally be performed separately and downstream using 
screens or other classifiers. Seed material can be produced by grinding. 
The process according to the invention is generally carried out as follows: 
firstly, the dextrin is dissolved in water. The alcohol is added to the 
aqueous dextrin solution, homogenization of the solution by intensive 
mechanical mixing having proved to be useful. The alcohol content of the 
solution has an upper limit due to the alcohol-soluble critical 
concentration. The solution is spray-granulated in a fluidized bed (with 
constant agitation). 
With appropriate choice of parameters, the granules forming, owing to the 
shell-like growth, are very compact, microporous and of uniform shape, so 
that they satisfy the highest requirements of abrasion resistance of 
granules. However, granules of high porosity can also be produced by 
suitable agglomeration conditions (low binder content), if agglomerates 
having rapid dispersion behaviour are required. 
The resulting granules have an alcohol content of 2 to 40, preferably 20 to 
30, % by weight and particle diameters of 0.1 to 3, preferably 0.2 to 2 
mm. The width of the particle diameter distribution (90% of the weight) is 
generally .+-.500, preferably .+-.200, .mu.m, based on the maximum of the 
(weight) distribution curve. 
In addition to alcohol and starch, natural and nature-identical flavourings 
can also be added to the granules, in which case the flavour content is 2 
to 30%, preferably 5 to 20%, based on granules. 
If appropriate, the alcohol-containing granules are then coated with a 
support material, which further improves the alcohol encapsulation quality 
and also the flowability and abrasion resistance. Suitable coating 
materials are simple and modified starches, gelatin, cellulose and 
cellulose derivatives, lactose, fats, waxes and the like. The proportion 
of the coating material is 5 to 70, preferably 5 to 30, % by weight, based 
on the uncoated granules. 
The alcohol-containing granules are abrasion-resistant, of low dust content 
and free-flowing. In contrast thereto, in spray-drying generally, solid 
particles are obtained in pulverulent form having elevated dust contents 
and markedly poorer flowability. The alcohol-containing granules produced 
by the process according to the invention can serve as additive for a 
multiplicity of pulverulent foods (for example dry soups, sauces, 
desserts, beverages etc.). 
The percentages in the following examples are in each case by weight. 
EXAMPLES 
The starches characterized in Table 1 were used in these examples. 
TABLE 1 
______________________________________ 
Composition of the hydrolyzed starches used 
(figures in % by weight) 
Degree of polymerization of glucose 
Type G.sub.1 
G.sub.2 
G.sub.3 
G.sub.4 
G.sub.5 
G.sub.6 
G.sub.7 
G.sub.8 
G.sub.9-n 
______________________________________ 
A 1.0 5.7 8.7 6.7 7.2 8.3 6.4 4.0 52.0 
B 10.0 5.2 7.9 6.1 6.5 7.5 5.8 3.6 47.4 
______________________________________ 
The symbol G signifies the glucose and the index signifies the degree of 
polymerization. The alcohol content of the granules is specified in the 
present invention in % by weight; the alcohol yield specifies the 
percentage proportion of the alcohol remaining in the granules, based on 
the amount of alcohol used in the solution employed. The alcohol content 
was determined by gas chromatography and the water content was determined 
by Karl-Fischer titration. 
The use of the hydrolyzed starch A, in which the content of saccharides 
having a degree of polymerization of glucose of up to 2 is 6.7%, primarily 
serves to show that, using the process according to the invention, despite 
a higher content of saccharides having a degree of polymerization of 
glucose of 2 in the hydrolyzed starch B, the alcohol content of the 
granules and the alcohol retention even increase. 
Example 1 
In a granulation apparatus of the type shown in European Patent 
Specification 332 031 and EP-A 163 836 and having the following features 
(diameter of the gas-distributor plate: 225 mm, atomizing nozzle: 
two-component nozzle, classifying discharge: zig-zag classifier, filter: 
internal bag filter) a solution consisting of 25% by weight of water, 25% 
by weight of ethanol and 50% of hydrolyzed starch (B as in Table 1) is 
granulated. The solution is sprayed at a temperature of 30.degree. C. into 
the fluidized-bed granulator. To fluidize the bed contents, nitrogen is 
blown in at a rate of 110 kg/h. The inlet temperture of the fluidizing gas 
is 105.degree. C. The temperature of the exhaust gas is 58.degree. C. The 
classifying gas fed is likewise nitrogen, at a rate of 10 kg/h at a 
temperature of 30.degree. C. The contents of the fluidized bed are 800 g. 
The granulation rate is 3 kg per hour. Free-flowing granules having a mean 
particle diameter of 600 .mu.m are obtained. The mean composition of the 
granules is: 29.1% ethanol, 4% water. This corresponds to an alcohol yield 
of 87% Alcohol and water contents remain constant over an experimental 
period of approximately 7 hours. On account of the constant pressure drop 
of the filter and the likewise constant bed contents, steady-state 
conditions with regard to the granulation process may be assumed. 
Example 2 (Comparison) 
In a pilot-plant spray tower, a spray solution which has the same 
composition as in Example 1 is dried at a feed air temperature of 
180.degree. C. and an exhaust air temperature of 75.degree. C. The 
resulting product contains only 17% alcohol, i.e. the alcohol 
encapsulation, at an alcohol yield of only 52%, was only 59% of the 
alcohol yields achieved by fluidized-bed spray granulation. Furthermore, 
the product is not dust-free, has a tendency to agglomeration and is thus 
of poor flowability. 
Example 3 
In the apparatus described in Example 1, a solution consisting of 25% 
water, 25% ethanol and 50% hydrolyzed starch (A as in Table 1) is 
granulated. The solution is sprayed at a temperature of 30.degree. C. into 
the fluidized-bed granulator. To fluidize the bed contents, nitrogen is 
blown in at a rate of 110 kg/h. The inlet temperature of the fluidizing 
gas is 105.degree. C. The temperature of the exhaust gas is 58.degree. C. 
The classifying gas fed is likewise nitrogen at a rate of 9 kg/h and a 
temperature of 30.degree. C. The contents of the fluidized bed are 600 g. 
The granulation rate is 2.5 kg per hour. Free-flowing granules having a 
mean particle diameter of 400 .mu.m are obtained. The mean composition of 
the granules is 25.4% by weight of ethanol, 4.2% of water. This 
corresponds to an alcohol yield of 77%. Remarkably, but at a lower content 
of saccharides having a degree of polymerization of glucose of up to 2 in 
the hydrolyzed starch used, lower alcohol contents and thus a poorer 
alcohol yield, in comparison with Example 1, are achieved. 
Example 4 
In the apparatus described in Example 1, a solution consisting of 25% 
water, 25% ethanol and 50% CAPSULE 1450.RTM. (starch octenyl succinate) is 
granulated. The solution is sprayed at a temperature of 30.degree. C. into 
the fluidized-bed granulator. To fluidize the bed contents, nitrogen is 
blown in at a rate of 110 kg/h. The inlet temperature of the fluidizing 
gas is 105.degree. C. The temperature of the exhaust gas is 52.degree. C. 
The classifying gas fed is likewise nitrogen at a rate of 10 kg/h and a 
temperature of 30.degree. C. The contents of the fluidized bed are 800 g. 
The granulation rate is 2.5 kg per hour. Free-flowing granules having a 
mean particle diameter of 1 mm are obtained. The mean composition of the 
granules is 26.8% ethanol, 2.5% water. This corresponds to an alcohol 
yield of 81%. 
Example 5 
In the apparatus described in Example 1, a solution consisting of 23.5% 
water, 30% natural rum flavouring (containing approximately 79% alcohol) 
and 46.5% hydrolyzed starch (B as in Table 1) is granulated. The solution 
is sprayed at a temperature of 35.degree. C. into the fluidized-bed 
granulator. To fluidize the bed contents, nitrogen is blown in at a rate 
of 110 kg/h. The inlet temperature of the fluidizing gas is 105.degree. C. 
The temperature of the exhaust gas is 52.degree. C. The classifying gas 
fed is likewise nitrogen at a rate of 8.5 kg/h and a temperature of 
52.degree. C. The contents of the fluidized bed are 200 g. The granulation 
rate is 3.5 kg per hour. Free-flowing granules having a mean particle 
diameter of 400 .mu.m are obtained. The mean alcohol content of the 
granules is 26.7% ethanol. This corresponds to an alcohol yield of 81%. 
Although virtually 30% water was present in the solution, surprisingly, 
high alcohol yields were achieved without change. 
Example 6 
In the apparatus described in Example 1, a solution consisting of 38% red 
wine concentrate (14.2% ethanol, 14.7% dry matter), prepared by reverse 
osmosis, 14% ethanol and 48% hydrolyzed starch (B as in Table 1) is 
granulated. The solution is sprayed at a temperature of 35.degree. C. into 
the fluidized-bed granulator. To fluidize the bed contents, nitrogen is 
blown in at a rate of 110 kg/h. The inlet temperature of the fluidizing 
gas is 105.degree. C. The temperature of the exhaust gas is 62.degree. C. 
The classifying gas fed is likewise nitrogen at a rate of 8.0 kg/h and a 
temperature of 57.degree. C. The contents of the fluidized bed are 450 g. 
The granulation rate is 2.8 kg per hour. Free-flowing granules having a 
mean particle diameter of 500 .mu.m are obtained. The mean alcohol content 
of the granules is 24.8% ethanol. This corresponds to an alcohol yield of 
70%. 
Example 7 
In the apparatus described in Example 1, a solution consisting of 28.3% 
water, 1.2% nature-identical brandy flavouring, 23.5% ethanol and 47% 
hydrolyzed starch (B as in Table 1) is granulated. The solution is sprayed 
at a temperature of 35.degree. C. into the fluidized-bed granulator. To 
fluidize the bed contents, nitrogen is blown in at a rate of 110 kg/h. The 
inlet temperature of the fluidizing gas is 105.degree. C. The temperature 
of the exhaust gas is 60.degree. C. The classifying gas fed is likewise 
nitrogen at a rate of 10.0 kg/h and a temperature of 40.degree. C. The 
contents of the fluidized bed are 800 g. The granulation rate is 2.9 kg 
per hour. Free-flowing granules having a mean particle diameter of 500 
.mu.m are obtained. The mean alcohol content of the granules is 25.1% 
ethanol. This corresponds to an alcohol yield of 73%.