Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
447-46 CIP
POLYDE~TRO~:E PRODUCT_AND PROCESS
ACRGROlJND OF T~IE INVENTION
This is a Continuation-in-part application of U.S.
Application Serial No. 881,612 filed May 12, 1992. The
present invention relates to a new process for producing
polydextrose and the product prepared thereby.
Polydextrose is a non-sucrose, essentially non-
nutritive carbohydrate substitute. Polydextrose can be
prepared through polymerization of glucose in the
presence of polycarboxylic acid catalysts and polyols.
Generally, polydextrose is known to be commercially
available in three forms: polydextrose A and
polydextrose K, which are powdered solids, and
polydextrose N supplied as a 70% solution. Each of these
products also contain some low molecular weight
components, such as glucose, sorbitol and certain
oligomers.
Most of the interest in polydextrose has centered
around its use in various edible compositions. For
example, polydextrose has stimulated interest in the food
arts as a low-calorie bulking agent or as a part of many
low-calorie or light foods since it has only about one-
quarter of the calories of sucrose. Non-~ood related
uses for the material have largely been ignored~
Unfortunately, the ability to disperse polydextrose
and use it in different products has been limited by
certain physical and chemical phenomena. Unlike most
saccharide products, it is relatively unreactive and
physically resistive to mixing and dispersing. While
artisans have be~n able to process sugar to enhance its
utility in food and other products, polydextrose
heretofore did not appear to be as versatile.
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Moreover, certain difficulties are incurred in the
production of polydextrose which create inefficiency and
waste and contribute to its lack of versatility as a
commodity. U.S. Patent Nos. 3,766,165 and 3,876,794
describe a method ~or making polydextrose. Generally,
polydextrose is manufactured by anhydrous melt
polymerization of glucose and maltose using edible acids
as catalysts and as cross-linking agents. The polymer
produced from the reaction is cooled, crystallized and
milled. Milling of the solidified polymer results in
loss of product in the form of unwanted fines which are
produced during milling. It is believed that up to 20%
of the product can be lost as a result of the production
of fines. Moreover, milling is an energy-intensive
procedure which detracts from the overall efficiency of
the process for manufacturing polydextrose, and the form
of the product is limited to ground solid polymer, which
is usually a powder. Thus, the present process for
manufacturing polydextrose for commercial sale and use is
severely limited.
In commonly-owned copending applications Serial No.
881,603 filed May 12, 1992 a process for producing a
modified polydextrose is disclosed wherein solid
polydextrose is spun in a cotton candy type machine to
provide a solid polydextrose product which is different
from the solid polydextrose feedstock. Similarly, parent
U.S. application Serial No. 881,612 filed May 12, 1992
describes a pharmaceutical composition made from a solid
polydextrose feedstock and a medicament. The resulting
composition is a second solid which has been transformed
by spinning a first solid polydextrosa feedstock
manufactured by the procedure set ~orth above, i.e., by
milling a solid polymer.
Other references which disclose processing by
spinning a solid feedstock are commonly-assigned U.S.
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Patent No. 4,855,326 and U.S. Patent No. 4,873,085, both
issued to Fuisz. These patents are directed to products
which include various active agents, having
pharmacological and/or cosmetic properties, combined with
readily water-soluble melt-spinnable materials such as
sugars or cellulosic substances. The active agents spun
with these materials demonstrate enhanced solubility.
Other disclosures are commonly-assigned U.S. Patent
Nos. 5,011,532 and 5,096~492 which contain examples where
oleaginous substances are mixed with sugar and melt-spun.
The spun products disperse readily in water, forming
colloidal or pseudo-colloidal dispersions. The '532
patent explains how oleaginous substances such as
vegetable oil, mineral oil, baby oil, margarine, lanolin,
cocoa butter and the like, which characteristically have
little or no affinity for water, can be rendered
dispersible by mixing the oleaginous substance with sugar
and melt-spinning the mixture in a cotton candy spinning
machine or equivalent.
Other disclosures dealing with spinning substances
with one or more sugars will be found in commonly-
assigned U.S. Patent Nos. 4,873,085; 4,997,856; 5,028,632
and 5,034,4~1. Generally, each of these disclosures are
~directed to melt-spinning sugar by introducing sugar and
various ingredients into a cotton candy spinning machine.
Such eguipment is normally operated at a temperature of
around 200C and at speeds of about 3,500 r.p.m. Melt-
spinning in such equipment relies upon certain
characteristics of sucrose, such as high crystallinity
and high physical and chemical lability. The spun
products disclosed in these patents and described as
taking the form of a floss or mass of spun fibers.
The disclosures set forth above relate to
transforming a solid feedstock material having a first
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structure to a second solid having a structure which is
altered from the first structure. None of these
disclosures addresses the difficulties incurred in
producing polydextrose as a commercial commodity.
It is, therefore an object of the present invention
to provide a process for overcoming some of the
shortcomings found in present polydextrose manufacturing
procedures and the products resulting therefrom. Other
and further objects will become known to those skilled in
the art as the invention is described herein.
S~RY OF T}I~3 INVEN~ION
The present invention is a process for manufacturing
polydextrose by subjecting flowable polydextrose
feedstock to flash shPar under conditions which provide
instantaneous formation of separate masses of solid
polydextrose. "Flowable polydextrose feedstock" results
directly from a polydextrose polymerization reaction and
is maintained in flowable condition without
solidification. As used herein "flowable polydextrose
feedstock" means that the polymer has not yet been
solidifiQd or crystallized before disrupting by use of
flash shear.
Polymerizate is used in the present application to
mean the product of a polymerization reaction which has
not und@rgone solidification. Polymerizate includes
solid product resulting from the process as well as
product in free-flow condition after it has been
disrupted by shear.
One embodiment of the present invention contemplates
subjecting the feedstock to flash shear by directing it
from the polymerization reactor to a spinning apparatus,
s~ch as a cotton candy type spinning machine, which
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provides shear force and separation whereby separate
polydextrose masses are formed.
In an alternative embodiment, ~lash shear is
provided by directing the new polydextrose feedstock
stream under pressure to an exit orifice. A disruptive
fluid shear force is applied to the feedstock stream to
separate it and permit it to solidify in the multiple
masses of polydextrose matrix.
In all embodiments ~lowable polydextrose feedstock
is maintained in the flowable state from polymerization
reaction to flash shear. Accordingly, it may be
necessary to provide apparatus to provide added heat
under controlled conditions to ensure maintenance of
flow.
In a preferr~d embodiment of the present invention
an additional ingredient may be introduced to the
polymerizate prior to subjecting it to shear. For
example, the additional ingredient or ingrPdients can be
injected into the stream after the polymerization
reaction. It is also contemplated that the additional
ingredient or ingredients can be incorporated before or
during polymerization. Additional ingredients include,
but are not limited to, oleaginous material, ~lavors, and
fragrances.
~he present invention also contemplates a new
polydextrose polymerizate which is prepared directly from
a flowable polydextrose stream resulting from a
polymerization reaction. The product is a discontinuous
polydextrose matrix having a morphology resulting from
subjecting the ~lowable feedstock to shear conditions
which provide separate masses of solid polydextrose
matrix. It is also contemplated that at least one - -
additional inyredient (or more than one ingredient) can
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be added while in the flowable stage. Alternatively, at
least one additional ingredient can be added prior to or
during the pol~merization reaction.
Yet another aspect of the invention is an apparatus
for manufacturing new polydextrose polymerizate which
includes a reaction chamber having means ~or controlling
the temperature, pressure, and moisture content of the~
polymerization reaction environment within the chamber,
and a means for advancing contents of the chamber
therefrom. The apparatus also includes means for
conveying the contents of the polymerization chamber
which is in fluid communication therewith. The means for
conveying also has the capability of controlling the
conditions o~ temperature, pressure and moisture as the
contents i5 moved through the conveyance means. Finally,
the apparatus includes a means for shearing polydextrose
melt and permitting free-flow formation of discreet
masses of polydextrose polymerizate.
As a result o~ the present invention, a commercial
polydextrose product can be provided without undergoing
the requirement of high intensity milling which is
necessary to reduce solid polymer to a flowable powder.
Consequently, the loss of fines, ger.erally associated
with milling, is eliminated. In addition, the morphology
of the solid particle produced can be changed by
controlling processing conditions.
Furthermore, a useful polydextrose product is formed
which can be readily used without further processing
alone or in combination with other ingredients. The
applications for these polydextrose containing materials
are vast.
As a consequence, polydextrose can be readily
supplied without need ~or the energy-intensive and
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inefficient procedur~c normally associated with
manufacturing of polydextrose.
As another advantage, polydextrose polymer can be
provided in the form of a shearform product without
requiring addition of heat sufficient to reduce a solid
product to flowable condition.
For better understanding of the present invention,
together with other and further objects, reference is
made to the following description, taken in conjunction
with the accompanying drawings, and its scope will be
pointed out in the appended claims.
15 BRIEF DESCR:CPTION OF THE DRAWINGS
Preferred embodiments of the invention have been
chosen for purposes of illustration and description, ~ut
are not intended in any way to restrict the scope of the
present invention. The preferred embodiments are shown
in the accompanying drawings, wherein:
Figure 1 is a block diagram of the process and
apparatus of the present invention;
Figure 2 is 2 schematic representation of one
embodiment of the process and apparatus of the present
invention;
.
Figure 3 is a schematic drawing of yet another
embodiment of the process and apparatus of the present
3S invention; and
Figure 4 is a schematic drawing of a shear nozzle
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which c~n be use~ in the embodiment shown in Fiaure 3.
DETAILED l)ESCRIPTION OF THE INVENTION
The present invention is a process for manufacturing
a polydextrose product which can be readily sold and used
as a commercial commodity. The produc~ is prepared by
subjecting a stream of polydextrose directly from a
polydextrose polymerization reaction to a shear force
which separates the stream into multiple masses of
polydextrose matrix under conditions which induce
solidification under free flow condition immediately
a~ter shearing.
Glucose and maltose polymers, commonly referred to
as polydextrose, are produced directly from glucose and
maltose by a process of anhydrous melt polymerization
using edible acids as catalysts and as cross-linking
agents. The starting materials used in the melt
polymeriæation are maltose or glucose, although other
simple sugars may be used as well. The sugars are
provided to the process as anhydrides or dry hydrated
solids, and are in powdered form.
The acids used as catalysts, cross-linking agents or
polymerization activators may be any one of a series of
xelatively non-volatile, edible, organic polycarboxylic
acids. It has been found that the following acids are
useful as polymerization activators: citric, fumaric,
tartaric, succinic, adipic, itaconic or terephthalic
acids. The acid or anhydride must be food-acceptable,
that is palatable and free of significant adverse affect
at the level of ordinary use. Inorganic acids are not
suitable for use as acid catalysts in anhydrous
polymerization since they do not serve as cross-linking
agents in the production of insoluble polyde~trose. The
acid selected should be relatively non-volatile, since
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more volatile acids mav be vaporized during the heating
and melting procedures which occur during polymerization.
The polycarboxylic acids used are largely, but
incompletely, esterified with the polydextrose in the
polymerizing process, forming acid polyglucose esters or
acid polymaltose esters.
The acid moieties are likely to serve as cross-
linking agents between different polyglucose or poly-
maltose molecules in the insoluble polymers whereas, inthe soluble polymers, each acid moiety is more likely to
be esterified to only the polymer molecule.
The dry powdered glucose can be combined with the
proper amount of acids. The acid and glucose or maltose
can be heated and melted under reduced pressure. The
melt should then be maintained in the absence of water
until substantial polymerization occurs. The anhydrous
melt polymerization should be ~arried out at pressures
below atmospheric, preferably not to exceed 300 mm. Hg,
e.g. from about 105 to 100 to 300 mm. Hg, and can be
obtained by the use of a vacuum pump, a steam jet
ejector, an aspirator or by other means. Air should be
excluded from the en~ironment of the polymerization
mixture in order to minimize decomposition and
discoloration of th~ polyglucoses or polymaltoses formed
in the polymerization. A fine stream of nitrogen has
been ~ound to be useful as a method for excluding air and
removing the waters of hydration and polymerization which
are formed. ~here the nitrogen purge is used, the vacuum
requirements are lessened, but pressures of 100 to 300
mm. Hg or less ara still preferred.
The duration of the reaction and the reactant
temperature are interdependent variables in the operation
of the polymerization. A preferable temperature for the
melt polymerization is from about 140C to about 180~C.
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The precise temperature for the anhydrous melt
polymerization depends on the initial ratio of glucose,
maltose or other sugars to the acid which is used, the
raaction time and the proportion of soluble polydextrose
to insoluble, cross-linked polydextrose which is desired
in the final product mixture.
The production of a large proportion of soluble
glucose or maltose polymers usually requires a
concentration of acid catalys~ between about 0.1 and 10
mole ~. Preferably the concentration is between 0.5 and
5~. As the amount of acid is increased, the degree of
acid cross-linking increases and the proportion of water- -
insoluble polyglucose or polymaltose increases. Where
acid concentrations are unnecessarily high, problems may
arise with regard to neutralizing the excess acid which
is present in the ~inal product mixture. The amount of
acid required for a particular polymerization, the
polymerization duration, the polymerization temperature
and the nature of the products desired are all
interdependent. The selection o~ the amount of acid to
be used should taXe into account these factors.
The thermal exposure ~reaction time and temperature)
used in the production of soluble polydextrose by
polymerization should be as low as possible, since
discoloration, caramelization and degradation increase
with prolonged exposure to high temperature. With regard
to the polymerization reaction, it is beneficial that as
the temperature of the polymerization is increased, the
time required to achieve substantially complete
polymerization decreases. Therefore, the polymerization
may be conducted at about 160'C and at a reaction
duration of about 8 hours, as well as at a temparature of
about 140C and a reaction duration of about 24 hours
with approximately the same resulting desree of
polymerization. Comparable results are also achieved in
continuous polymerization at te~peratures in the range of
about 200O to 3000C in about 10 minutes or less without
significant darkening while the reaction is under vacuum.
With regard to production of insoluble polydextrose,
the molar ratio of glucose or maltose to acid may also be
within the ranges specified above for production of
soluble polysaccharidas, and especially from about 2.5 to
about 10 mole % of acid. It is preferable, to use molar
ratios of glucose or maltose acid of between about 12:1
to about 20:1 in the production of insoluble
polydextrose. These ratios are preferred in spite of the
requirements of high reaction temperature and relatively
long reaction times because the total yield of soluble
and insoluble polydextrose is between 90 and 99% at the
sugar to acid ratios. Thus, using these higher ratios,
it is possible to produce in one reaction mixture a yield
of between 50 and 60% of insoluble polydextrose and
between about 40 and 50~ of soluble polydextrose.
It is important that the time reguired to introduce
the stream of new polydextrose feedstock to shear be
minimized in order to reduce the possibility of browning,
charring, or caramelization. Thus, the means for
~5 directing the feedstock stream from the reactor to the
shear step must be heated and configured to minimize the
residence time of exposure to high temperature.
It has also been found that inclusion of a food
acceptable polyol, such as sorbitol, in the saccharide-
carboxylic acid reaction mixture prior to
polycondensation yields a superior product. In most
cases, 90~ or more of the polyol cannot be isolated from
the condensation product, demonstrating that it has been
chemically incorporated in the polymer. These additives
function as internal plasticisers to reduce viscosity and
also to provide improved color and taste. This is
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evident for example in the manufacture of hard candy from
such condensation polymers, where the rheological
propertias of the melt are improved during processing.
Foaming is minimized and a better tasting product of
lighter color is obtained. In addition to sorbitol,
other food-acceptable polyols including glycerol,
erythritol, zylitol, mannitol and galactitol. Polyol
concentrations of from about 5 to 20% by weight of the
total reaction mixture provide such advantages, and
levels of from about 8 to 12% by weight are preferred.
Chemical purification is not required for products
made in accordance with the process of the present
invention. Where soluble and insoluble polydextroses are
produced together, separation may be desired.
Neutralization of the polydextrose may be desirable
for certain applications despite the very low levels of
acid catalyst employed. For example, where the
polydextrose are to be used in dietetic foods containing
whole milk, excess acid which may be present and thP
unneutralized polydextrose will tend to curdle the milk.
In th~ case of soluble polydextrose, the solutions of
polydextrose are neutralized directly. This
neutralization may ba accomplished by adding carbonates
of potassium, sodium, calcium or magnesium to the
solution of polydextrose. Where sodium and potassium are
used together a physiologically balanced mixture may be
used. ~he salt content of a typical polydextrose
solution which has been adjusted to a pH of about 5 to 6
is a mere 0.5 to 1.0~ Other materials which may be used
to adiust the pH of soluble polydextrose solutions
include l-lysine, d-glucosamine, N-methyl glucamine and
am~onium hydroxide. The first two of these compounds are
natural materials and should not be objectionable as an
ingredient of dietetic foods and the last compound, which
is rapidly excreted by the body in the form of urea,
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would not be objectionable as an ingredient in dietetic
foods. N-methyl glucamine is used as solubilizing agent
for pharmaceuticals and should not be objectionable as an
ingredient in dietetic foods. Other methods for reducing
the acidity of polydextrose solutions are dialysis and
ion exchange.
Most of the polydextroses produced in this invention
have an average molecular weight of from about 1,500 to
about 36,000. The soluble polyglucoses which are
produced have been found to have an average molecular
weight of from about 1,500 to about 18,000 and the
insoluble polydextroses produced have been found to have
an average molecular weight o~ between about 6,000 and
about 36,000.
The experim~ntally determined number average
molecular weights of the polydextroses produced in this
procedure are usually found to range from about 1,000 to
about 24,000, with most of the molecular weights falling
in the range of 4,000 to about 12,000. These number
average molecular weights were determined by the modified
reducing end-group method according to Isbell (J.Res.
Natl. Bur. Standards 2~, 241 (1940~). This method is
based on the reduction of alkaline copper nitrate
reagent. The number average molecular weight values are
computed on the basis of standardization with
gentiobiose, assuming that equimolar quantities o~
polydextrose and gentiobiose have approximately the same
reducing power and assuming one reducing end-group per
molecule.
The linkages which predominate in the polydextrose
are primarily 1-6 but other linkages also occur. In the
soluble polyglucoses each of the acid moieties is
esterified to polyglucose. Where the acid moieties is
esterified to more than one polyglucose moiety, cross-
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linking results.
The soluble polydextroses are useful for imparting
physical properties of natural foods, other than
sweetness, to dietetic foods from which natural sugars
have been removed and replaced by artificial or other
sweeteners. In ~aked goods, ~or example, the new
polydextrose affect rheology and texture in a manner
analogous to sugar and can replace sugar as a bulking
agent. Typical uses for the soluble polydextroses are
found in low calorie jellies, jams, preserves, marmalades
and fruit butters, in dietetic frozen food compositions
including ice cream, ice milk, sherbet and water ices; in
baked goods such as cakes, cookies, pastries and other
foodstuffs containing wheat or other flour; in icings,
candy and chewing gum; in beverages such as non-alcoholic
so~t drinks and root extracts; in syrups; in toppings,
sauces and puddings, in salad dressings and as bulking
agents for dry low calories sweetener compositions
containing cyclamate or saccharine.
The use of polydextrose provided by this invention
allows the elimination of 20 to 100% of the normal fat,
oil or fatty triglyceride components of the food. The
degree of fat, oil or fatty triglyceride elimination will
naturally vary with the type of food, for example, in a
french salad dressing it is possible to completely
eliminate the oily component normally included. In
chocolate coatings, ice rream mixes and whipped toppings,
20 to 80% of the fat, oil or triglyceride can be
eliminated while still retaining the required foqd
characteristics such as texture, gloss, ~iscosity and
taste of the food product.
As previously mentioned, aside from the replacement
of sugar in many recipes there is an appreciable flour
sparing and/or fat sparing effect that is possible
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without decreasing the quality of the food. The result
is a further reduction in total calorie value of the
foo~.
The term "fatty-triglyceridel' refers to ~lycerol
esters of the higher fatty acids contained in fats and
oils. The use of the soluble polydextroses allows
elimination of at least part of the fatty-triglyceride
component of food. The degree of fatty-triglyceride
elimination will naturally vary with the type of ~oodO
In other types of food products, at least part of
the carbohydrate ordinarily contained is replaced by
soluble polydextroses. Also in some products at least
part of the fatty-triglyceride and substantially all of
the carbohydrate ordinarily contained is replaceable by
soluble polydextrose.
The so-called fat-sparing effect is possible without
decreasing the quality of the food in that the required
food characteristics such as texture, gloss, viscosity
and taste are still retained. Furthermore, the caloric
value of these foods is lowered considerably by the fact
that soluble polydextroses have been used to replace
sugars and fatty-triglycerides which are contained in the
natural counterparts of the dietetic foods.
In the traditional production of polydextrose, crude
polymer was taken ~rom ~he polymeriza~ion reaction and
milled in order to provide a flowable powder useful in
production of food products. This procedure has been
described in U.S. Patent No. 3,876,794 and U.S. Patent
No. 3,766,165. This ~illing procedure produces unwanted
fines which are lost and/or discarded in order to provide
polydextrose as a commercial commodity.
In the present invention, however, the contents of
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the reaction chamber is directed to a spinning h~ad which
includes a circumferential wall having openings through
which feedstock can pass under centrifugal force as
separate and distinct masses o~ polydextrose. The
feedstock is metered to the spinning head at a rate which
permits this polymerizate to be forced against the
circumferential wall and permit separation of discrete
portions of the mass as the feedstock melt is exposed to
an opening in the wall. A heating element can be
provided to maintain the polymer in flowable condition.
A preferred embodiment contemplates the use of a heating
element which provides controllad heating. The discrete
masses are then cooled to form a solid product having the
shape of flaXes, fibers, spicules and other generally
non-descript physical form which result from
eolidification while in free flow condition.
In an alternative embodiment, the molten material
can be directed to a chamber in which the product is
moved l~nder pressure tc an exit orifice. A stream of
polydextrose is forced through the orifice and is
subjected to a stream of fluid, gas or liquid, impacting
the ~eedstock at a velocity which creates flash shear
force. Apparatus with controlled heating can be used to
maintain the flowability of the polymer from reactor to
exit orifice. The force created by fluid impinging
against the feedstock is referred to as disruptive fluid
~hear force.
Presently, the preferred fluid is air. However, the
invention is not limited to the type of fluid used to
create the disruptive fluid shear force.
In one embodiment, air is directed against the
feedstock as a continuous high velocity jet. Another
embodiment contemplates propelling the feedstock at high
velocity against the force of an air atmosphere. In both
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cases the feedstocX is abruptly disrupted into discrete
discontinuous masses due to shear acting on the feedstock
material while it has internal flow~
In the a~ove flash shear process, a rapid cooling
step is preferably used immediately following the
shearing of the molten material into discrete masses to
reduce discoloration or degradation. Preferably the
discrete masses are immediately introduced into a cold
gaseous environment such as that produced by refrigerated
air, liquid carbon dioxide, liquid nitrogen and the like.
A characteristic of the product of the present
invention is that the matrix resulting therefrom has a
morphology which results from allowing flash disrupted
feedstock to re~orm during free ~low. This unique free-
flow formation is achieved by preventing hindrance of
continued flow while the material cooled to its original
matrix structure.
In order to provide the new matrix material of the
present invention, a unique apparatus has been devised
which is able to deliver the feedstock from a reactor $o
a point where it is subje~ted to shear while in the
internal ~low conditions.
In Figure 1 a block diagram is shown of the
apparatus of the present invention wherein a reactor 10
is connected for fluid flow to a directing means 20 which
maintains the contents of the polymerization reactant
chamber in fluid flow condition for the next step of the
apparatus. Finally, a means for applying shear force 30
is provided for shearing the feedstocX and providing the
novel polydextrose polymerizate.
In Figure 2 a schematic representation of one
embodiment of the invention has been shown wherein a
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reaction chamber 11 is provided for polymerizing the
polydextrose. In fluid communication ther~lth is a
trans~er means 21 which maintains the contents of the
reaction chamber in ~luid flow condition for shearingO
Finally, a means for shearing 31 is provided for receipt
of the polydextrose melt 22 therein. Specifically, the
shearing means 31 is a spinning head having openings 32
arranged around a circumferential wall 33 through which
the polydextrose is separated and flung outwardly under
centrifugal force during spinning. A heating element
such as a heating band or ribbon, can be provided around
the circumference of the head to maintain the
polydextrose in ~lowable condition.
Polydextrose moves under centrifugal force through the
heating element and opening 32 and is caught in a bin 34.
The bin 34 can be lowered by means of platform 35
arranged on lift means 36. The lift means 36 can be
raised and again positioned for receipt of polydextrose.
In Figure 3, a reaction chamber 12 is provided for
polymerizing polydextrose and is in direct fluid
communication wi~h a extruder feeder 23. The extruder
feeder 23 advances the contents of the reaction chamber
12 through to an exit connecting means 24. The extruder
and connecting means 24 control the temperature, pressure
and moisture content of the throughput before being
introduced to a nozzla 37 which provides the shearing
effect for producing the novel polydextrose polymerizate.
In order to provide disruptive fluid shear force, high
velocity heated air 38 is directed to the nozzle 37.
Referring to Figure 4, a stream of air 38 can be
seen being directed against the feedstoc~ e~terior of the
nozzle to provide discontinuities in the feedstoc~ and
permit a morphology to be achieved by free-flow
solidification as discontinuous masses. In Figure 4, the
air stream 38 is seen in fluid communication with annular
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2 ~
chamber 83 which surrounds the internal nozzle device 84.
Feedstock 22' is fed to the nozzle and exits as a
coherent stream 87 where it is subjected to high-velocity
air stream 85. The high-velocity air stream 85 is
craated by tortuous path exit route provided by air cap
80 and retaining ring 81.
Other measures can be taken to ensure that the
internal flow condition created in the extruder/heater is
not lost by heat transfer as the feedstock is advanced to
the point of shear and beyond to permit free-flow
formation. For example, valve mechanism 61 can be heated
to eliminate transfer of heat from the feedstock to a
relatively cooler valve mechanism. Moreover, heat can be
maintained at the point of shear, generally identified by
elements 80 and 81, by directing a heatgun at them during
operating or by using a temperature controlled heating
bandO Alternatively, the temperature of the internal
nozzle 84 can be raised or lowered relative to the stream
of heated air to prevent transfer of heat from the
feedstock and conseguent cooling below ~low conditions.
As the process continues, however, a steady-state
temperature of each of the mechanisms will be attained 50
that additional heat to individual elements of the
operations is not required to prevent undue heat transfer
and cooling.
When air is used to create the shear force, it is
applied in a two-fluid nozzle at a pressure of from about
1.5 to about 20 atmospheres. Preferably, the pressure is
applied at about 2 atmospheres to 10 atmospheres. The
temperature of the air used to create the shear force
should preferably be controlled to a te~perature at least
about 0.1C above the temperature of the feedstock being
ejected for every atmosphere of pressure.
Oleaginous material can be added before or after
\
-20- 21~ (ç~
polymerization. The oleaginous substance can be a food-
acceptable/edible oil. Such substances are selected from
vegetable oils, soybean oil, canola oil, corn oil,
sun~lower oil, olive oil, mixtures thereof and the like.
In this aspect, the oils are pre~erably low in saturated
fats.
The particles produced in the flash shear processes
generally have a morphology which differs from that of
the ground powders obtained in previous processes. The
flash shear polydextrose can be produced as flakes,
fibers, (including hollow fibers) and spicules.
The oleaginous~can be a fat such as an edible animal
~at or fatty material. For example, beef, pork, lamb or
similar animal fats or mixtures thereof may be used.
Similarly, fat containing materials such as beef tallow,
sheep tallow, butter or lards, hydrogenated animal and/or
vegetable oils may be included. Moreover, fish or
crustacean-based oils or oleaginous materials are also
useful Combinations of the above-described oleaginous
materials are also contemplated.
Another aspect of the pre~ent invention is the
ability to include at least one additional material with
the polydextrose such as bioaffecting agents. Categories
of such ingredients may vary widely. Illustrative
categor-es and specific examples include:
(a) Antitussives, such as dextromethorphan, and
chlorphedianol hydrochloride;
(b) Antihistamines, such as chlorpheniramine
maleate and terfenadine;
(c) Dacongestants, such as phenylephrine,
phenylpropanolamine, pseudoephedrine and
ephedrine;
(d) Various alkaloids, such as codaine and
morphine;
- .
~,' ' ' . '
~', ~ '
`' ~ ' ' " ' ' .
-21- 2 ~ 3 c~ ~ ~' &
(e~ Mineral supplements such as potassium chloride,
(f) Laxative, vitamins and antacids;
(g) Ion-exchange resins s~ch as cholestyramine;
(h) Anti-cholesterolemic and anti-lipid agents;
(i) Antiarrhythmics such as N-acetyl-procainamide;
(j) Antipyretics and analgesics such as
acetaminophen, aspirin and ibuprofen;
(k) Appetite suppressants such as
phenylpropanolamine hydrochloride or cafeine;
(1) Expectorants such as guaifenesin,
(m) Anti-anxiety agents such as diazepam; and
(n) Anti-ulcer agents such as sucralfate.
A non limiting list of other active ingredients
includes anti~inflammatory substances, coronary dilators,
cerebral dilators, peripheral vasodilators, anti-
infectives, psychotropics, antimanics, stimulants
gastrointestinal agents, sedatives, antidiarrheal
preparations, anti-anginal drugs, vasodialators, anti-
hypertensive drugs, vasoconstrictors, migraine
treatments, antibiotics, tranquilizers, antipsychotics,
antitumor drugs, anticoagulants, antithrombotic drugs,
hypnotics, anti-emetics, anti-nauseants, anticonvulsants,
neuromuscular drugs, hyper- and hypoglycemic agents,
~5 thyroid and antithyroid preparation, diuretics
antispasmodics, uterine relaxants, mineral and
nutritional additives, antiobesity drugs, anabolic drugs,
ery~hropoietic drugs, antiasthmatics, cough suppressants,
mucolytics, anti-uricemic drugs, and mixtures thereof.
The medicaments contemplated herein are particularly
well-suited for use when it is desired to disperse the
agent in aqueous liquids andJor mask cover the
undesirable tastes of actives. The flavor of unpleasant
medicaments can also be masked or altered i~ desired by
adding a flavoring agent and/or a sweetening agent to the
pre-spun mixture.
-22- 21~
In an alternative aspect of the invention, the
adjuvant materials included with the polydextrose are
cosmetic-related ingredients. Ccosmetic ingredients are
those materials which have a skin beautifying and/or
complexion-related activity. Such products can be used
externally on hair, skin or both. A non-limiting list of
ingredients which have appearance-improving cosmPtic
activity includes dimethyl siloxanes,
mucopolysaccharides, methyl and propyl parabens, biotin,
lanolin, aloe, glycerin, mineral oil, nicotinamide
compounds, sun screens, such as para-aminobenzoic acid,
hair conditions, moisturizers, moisturizing creams,
astringents, powders such as talcs and combinations
thereof.
It will be understood by those skilled in the art
from the present description that additional materials
can be included with the polydextrose and principle
active in~redients. Thus, colors, flavorants,
fragrances, dyes, pigments, antioxidants, preservatives
and similar ingredients can be added in both the matrix
and product in which the matrix is included. Such
materials ser~e to improve the appearance, aroma, shelf-
life or other properties of the produrts prepared and
described hsrein. ~oreover, the final products can also
contain those adjuvant materials which are particularly
suited for particular end uses.
Flavorants can include sweeteners, both synthetic
and natural, and other flavor ingredients, such as fla~or
oils or essences. These oils are generally deriYed from
plant extracts, although they may also be synthetically ~ -
derived. Peppermint oil. spearmint oil, cinnamon oil,
oil of wintergreen, citrus oils and other fruit essences
are the most commonly used flavor oils which are employed
in the present invention. Examples of citrus or first
oils and/or essences which are useful include a host of
- ~
.
~ ~ ~-3.
-23-
materials such as 2~ple, apricot, banana, blueberry,
cherry, grape, grapefruit, lemon, lime, orange, pear,
peaches, pineapple, plum, raspberry, strawberry and the
like. Mixtures and derivatives of these oils are
contemplated.
Additional flavorants can be chosen from synthetic
flavor oils and flavoring aromatics, and/or oils, oleo
resins and extracts derived from plants, leaves, flowers,
furits and so forth, and combination thereo~. For
example, clove oil, bay oil, anise oil, eucalyptus oil,
thyme oil, cedar leaf oil, oil of nutmeg, oil of sage,
oil of bitter almonds and cassia oil may be used.
Commonly used flavors include manthol, artificial
~anilla, cinnamon derivatives, and various fruit flavors,
whether employed individually or in admixtur~.
Flavorings such as aldehydes and esters including
cinnamyl acetate, cinnamaldehyde, citral diethylacetal,
dihydrocarvyl acetate, eugenyl formate, p-methylamisol,
and so forth may also be used. Generally any flavoring
or food additive such as those described in "Chemicals
Used in Food Processing," pub. 1274 by the National
Academy of Sciences, pages 63-258 may be used.
Further examples of aldehyde flavorings include, but
are not limited to acetaldehyde (apple~; benzaldehyde
(cherry, almond), anisic aldehyde (licorice, anise);
cinnamic aldehyde (cinnamon); citral, i.e., alpha citral
(lemon, lime); neral, i>e.'beta citral (lemon, lime);
decanal (orange, lemon); ethyl vanillin (vanilla,
cream),; hellotropine, i.e., piperonal (vanilla, cream);
vanillin (vanilla, cream); alpha-amyl cinnamaldehyde
(spicy fruity flavors); butyraldehyde (butter, cheese);
valcraldehyde (butter, chee~e); citronellal; decanal
(citrus fruits); aldehyde C-8 (citrus fruits); aldehyde
C-9 ~citrus fruits); aldehyde C-12 (citrus fruits); 2-
- . .. ; ~ . .
-24-
ethylbutyraldehyde (berry fruits); hexenal, i.e., trans-2
(berry fruits~; tolyl aldehyde (cherry, almond),
veratraldehyde (vanilla); 2,6-dimethyl-5-heptenal, i.e.
Melonal (melon); 2,6-dimethyl-5-heptenal, i.e. Melanal
(melon); 2,6-dimethyloctanal (green fruit); and 2-
dodecenal (citrus, mandarin); cherry; grape; strawberry
shortcake; mixtures thereof; and the like.
Other specific flavor compounds such as
ethylacetate, thiophene ethylpropionate, ethyl butyrate,
2-hexanoate, 2-methylpyazine, hiptaldehyde, 2-octanone,
limonene, and eugenol are useful.
The nature and amount of all materials included in
the matrix will vary greatly. The amount of active
material included in the product will depend upon the
active ingredient and ~he amount required to achieve a
desired therapeutic and/or cosmetic ~ffect.
In further aspects of the invention, supplemental
materials such as bioadhesives, dispersants, surfactants
and the like can be included. For example, bioadhesive-
type materials such as hydrogels or synthetic materials
such as polyvinyl-pyrrolidone are useful. Dispersants
such as polyacrylates and alginates are also useful.
A non-limiting list of surfactants which are useful
in combination with the matrix of the invention include
as follows: anionic surfactants such as alkyl `~
carboxylates, alkyl sulfates, ethoxylated alkyl sulfates,
sulfosuccinate esters, isothionates, sarcosinates, sodium
lauryl sulfoacetates, fatty acid-polypeptide condensates,
linear alkyl arylsolfonates (LAS), alpha-ol~fin
sulfonates ~AOS), organic phosphate esters; cationic
surfactants such as sodium lauryl sulfate (SLS),
cetrimonium bromide and polysorbates; amphoteric
surfactants such as alkylamino propionates, acyl
2~ 5~
-2~-
ethylenediamines and betaines; non-ionic surfactants such
as ethoxylated and propoxylated derivatives and polyol
esters including sorbitan esters polyoxyethylene ethers;
alkyl polyglycosides, sulfonic acid/linear alkylate
sul~onates, silicon derivad phosphate esters, non-oxynol
surfactans, Triton~ surfactants and alXylphenols.
The various ingredients added to the polydextrose
can be added ~y various means including introduction into
static mixers in the flow path or introduction into high
shear mixers in the flow path. Where the ingredient is
sensitive to degradation at the temperatures of the
molten polydextrose the ingredients are added just prior
to ~he flash shear step.
In a preferred embodiment wetting agents are added
~o ~he polydextrose prior the flash shear step,
preferably in amounts of less than 5~ by weight.
Particularly useful wetting agents include lecithin,
maltodextrins (including corn syrup solids), fructose,
ylucose, honey, hydrogenated honay, inositol, sucro~e,
sodium prryolidone carboxylic acid, lactic acids,
polyethylene glycols, glycerin, polyols such as,
propylene glycol, glycerol, sorbitol, mannitol, xylitol
and platinit and the surfactants mentioned above. The
discrete particles made with such wetting agents have
improved dispersibility especially when large volumes of
polydextrose are added to aqueous medium~ In many
instances clumping of the dry solids often encountered
with polydextrose solids is substantially eliminated.
The ~ollowing examples serve to provide further
appreciation of the invention, but are not meant in any
way to restrict the ef~ective scope of the invention. In
examples in which spinning is used, reference is made to
copending com~only-owned U.S. Application Serial No.
954,257, filed September 30, 1992 and in general
.. ..... . . .
-26- 2~
apparatus such as those adapted to produce cotton candy
or floss from sugar. Illustrative of such machine is the
Econo Floss Nachine Model 3017 manufactured by Gold Metal
Products Company of Cincinnati, Ohio. It will be
appreciated by those skilled in the art that any
apparatus or physical process which provides similar
shear force and time/temperature gradient conditions can
also be used. Similarly, when disruptive fluid shear
force is mentioned, the phenomena described in copending
commonly-owned application bearing Serial No. 965,804
filed on October 23, 1992 is referred to. By reference
to these processes, the preferred embodiments of the
present invention can be better described.
PR~IMINARY ~XAMPLE
In order to ~erify the ability to produce a
shearform product from molten polydextrose, an experiment
was run wherein a melted stream of polydextrose was
directed from an extruder into a dual xibbon spinning
headO A white floss was produced which has excellent
color and texture characteristics.
The examples set forth herein describe full
implementation of the invention.
: - . ........................ .- - . . .
.
.:-~- , . .
- .
-27- 2~.15(~
EX~MPL S
Example
In this example, an insoluble polydextrose is
prepared which shall be referred to in subsequent
examples for purposes of explaining the process of the
present invention. In particular, dried white,
crystalline, refined dextrose (pure monosaccharide), in
anhydrous form and powdered citric acid are mixed at a
ratio of 16:1, and is reacted while stirring under a
pressure of 14 mm. of Hg. The melt is maintained at 170
centigrade for 25 hours in order to complete
polymerization. The charge resulting from this reaction
is used in further examples set forth herein to produce
the novel polymerizate resulting from the present
invention.
~xamPls 2
In Example 2 a water soluble polydextrose feedstock
is prepared by contacting powdered anhydrous glucose and
citric acid at a ratio of 39:1. The mixture is
intimately mixed and reacted at 160~ centigrade at a -
reduced pressure of 0.1 mm of Hg for 3 hours. This
product is used later as a charge for producing the novel
polymerizate of the present invention. -~
~xam~le 3
The reactor charge resulting from Example 1 is
directed ts a spinning apparatus operating at a speed o~
approximately 3500 RP~. The operating temperature o~ the
head is approximately 140 to lSO~centigrade. ~he molten
~aterial resulting from the polymerization reaction is
metered to the spinning head at a rate which permits the
material to be flung outwardly against the
, ; . . .. ~ . .. . _ .. ..... = . . ... . ... .. .. . . . . . . .......... ... .
- : : :~ . .~: , . .
. ~. , ~ . . : . . . . - . .
21~58~
-~8-
circumferential wall of the spinnin~ head and forced by
centrifugal force through openings provided in the head
to separate and permit free flow formation of discrete
polydextrose masses. The rate of introducing the
material to the head is such that it is not permitted to
solidify or crystallize before it completes the process
of the present invention.
White spicule-like flakes are expected as a result
0 of the present process. These flakes are easily handled
and readily dispersible in other masses such as food
ingredients.
E~amzle 4
~5
The contents of the reactor in Example 1 are in
fluid communication with a chamher which advances the
material throughput under pressure to a exit nozzle. The
reaction mixture is forced through the exit nozzle under
pressure to be met by a stream of heated high velocity
air which creates flash disruptive shear force on the
feedstocX. The ~lash disrupted feedstock is permitted to
form as discreet masses during free-flow to attain an
original polymerizate morphology.
The expected polydextrose polymerizate is
substantially white in color and has a light flaky
texture. This material is easily adaptable for many uses
and can be conveniently packaged as a commercial
commodity for distribution, sale, and use.
Example 5
The reactor charge resulting from Example 2 is
directed to a spinning appar~tus operating at a speed of
approximately 3500 RPM. The operating temperature of the
head is approximately 140 to 150-centigrade. The molten
. . .
; ~ ;
. . .
~':
. ~.
2~
-29-
material resulting from the polymerization reaction is
metered to the spinning head at a rate which permits the
material to be flung outwardly against the
circumferential wall of the spinning head and forced by
centrifugal force through openings provide~ in the head
to separate and permit free flow formation of discrete
polydextrose masses. A heating band is positioned
adjacent to the outer wall to provide the effective
extrusion orifice. The heating band is heated to
compensate for any cooling of the spinning apparatus and
to maintain an extrusion oriface at the flow temperature
of the polydextrose. The rate of introducing the
material to the head is such that it is not permitted to
solidify or crystallize before it completes the process
of the present invention.
White spicule-like flakes are expected as a result
of the present process. These flakes are easily handled
and readily dispersible in other masses such as food -
ingradients.
Example ~
The contents of the reactor-in Example 2 are in
fluid communication with a chamber which advances the
material throughput under pressure to a exit nozzle. The
chamber is provided with controlled heating to maintain
flowable conditions. The reaction mixture is forced
through the exit nozzle under pressure to be met by a
ctream of heated high velocity air which creates flash
disruptive shear force on the feedstock. The flash
disrupted feedstock is permitted to form as discreet
masses during free-flow to attain an original
polymerizate morphology.
The expe~ted polydextrose polymerizate is
substantially white in color and has a light flaky
- - . .:
. , - :- . . .
: :
2 ~
-30-
texture. This material is easily adap~able for many uses
and can be conveniently packaged as a commercial
commodity for distribution, sale, and use.
Thus, while there have been described what are
presently believed to be the preferred embodiments of the
present invention, those skilled in the art will realize
that other and further modifications can be made without
departing from the true spirit of the invention, and it
is intended to include all such modifications and
variations as come within the scope of the claims as set
forth below. "t
. - ' '
:: ,
.. .. .
