Note: Descriptions are shown in the official language in which they were submitted.
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WO 02/078737 PCT/US02/10025
GRANULE WITH REDUCED DUST POTENTIAL
BACKGROUND OF THE INVENTION
Recently the use of enzymes, especially of microbial origin, has become more
and
more common. Enzymes are used in several industries including, for example,
the starch
industry, the dairy industry, and the detergent industry. It is well known in
the detergent
industry that the use of enzymes, particularly proteolytic enzymes, has
created industrial
hygiene concerns for detergent factory workers, particularly due to the health
risks
associated with dustiness of the available enzymes.
Since the introduction of enzymes into the detergent business, many
developments
in the granulation and coating of enzymes have been offered by the industry.
See for
example the following patents relating to enzyme granulation:
U.S. Patent 4,106,991 describes an improved formation of enzyme granules by
including within the composition undergoing granulation, finely divided
cellulose fibers in an
amount of 2-40% w/w based on the dry weight of the whole composition. In
addition, this
patent describes that waxy substances can be used to coat the particles of the
granulate.
U.S. Patent 4,689,297 describes enzyme containing particles which comprise a
particulate, water dispersible core which is 150 - 2,000 microns in its
longest dimension, a
uniform layer of enzyme around the core particle which amounts to 10%-35% by
weight of
the weight of the core particle, and a layer of macro-molecular, film-forming,
water soluble or
dispersible coating agent uniformly surrounding the enzyme layer wherein the
combination
of enzyme and coating agent is from 25-55% of the weight of the core particle.
The core
material described in this patent includes clay, a sugar crystal enclosed in
layers of corn
starch which is coated with a layer of dextrin, agglomerated potato starch,
particulate salt,
agglomerated trisodium citrate, pan crystallized NaCl flakes, bentonite
granules or prills,
granules containing bentonite, Kaolin and diatomaceous earth or sodium citrate
crystals.
The film forming material may be a fatty acid ester, an alkoxylated alcohol, a
polyvinyl
alcohol or an ethoxylated alkylphenol.
U.S. Patent 4,740,469 describes an enzyme granular composition consisting
essentially of from 1-35% by weight of an enzyme and from 0.5-30% by weight of
a synthetic
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fibrous material having an average length of from 100-500 micron and a
fineness in the
range of from 0.05-0.7 denier, with the balance being an extender or filler.
The granular
composition may further comprise a molten waxy material, such as polyethylene
glycol, and
optionally a colorant such as titanium dioxide.
U.S. Patent 5,254,283 describes a particulate material which has been coated
with a
continuous layer of a non-water soluble, warp size polymer. U.S. Patent
5,324,649
describes enzyme-containing granules having a core, an enzyme layer and an
outer coating
layer. The enzyme layer and, optionally, the core and outer coating layer
contain a vinyl
polymer.
WO 91/09941 describes an enzyme containing preparation whereby at least 50% of
the enzymatic activity is present in the preparation as enzyme crystals. The
preparation can
be either a slurry or a granulate.
WO 97/12958 discloses a microgranular enzyme composition. The granules are
made by fluid-bed agglomeration which results in granules with numerous
carrier or seed
particles coated with enzyme and bound together by a binder.
However, even in light of these developments offered by the industry (as
described
above) there is a continuing need for low-dust granules. In particular, it is
especially
problematic in the detergent industry when granules in general, or those
comprising proteins
or enzymes, form dust and are aerosolized. In these cases, workers are often
exposed to
the contents of the granules and can develop severe allergic reactions.
Therefore, it is an
object of the present invention to provide a method of producing a low-dust
enzyme granule
by adding antifoam agent. It is a further object of the invention to
facilitate a safer
environment for workers in the detergent industry who are exposed to enzyme
containing
granules.
SUMMARY OF THE INVENTION
The present invention relates to a granule that has a reduced dusting
potential. The
granule of the invention is prepared in a process in which an antifoam agent
is added during
granule manufacture such that the antifoam agent is present in the resulting
granule in a
concentration sufficient to reduce the dusting potential of the produced
granule.
In one embodiment of the invention, a granule for use in solid formulations
comprises a seed particle; an admixture of an allergenic agent and antifoaming
agent
surrounding the seed particle; wherein the granule has at least 10% less dust
as measured
by a Heubach test than a granule without the antifoaming agent prepared by a
similar
process.
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In another embodiment of the invention, a granule for use in solid
formulations
comprises a seed particle; an admixture of an allergenic component and
antifoaming agent
surrounding the seed particle; a coating surrounding the admixture, the
coating comprising
an antifoaming agent and at least one barrier material, wherein the granule
has at least 10%
less dust as measured by a Heubach test than a granule without the antifoaming
agent
prepared by a similar process.
In yet another embodiment of the invention, a granule for use in solid
formulations
comprises a seed particle; an allergenic component surrounding the seed
particle; a coating
surrounding the allergenic component, the coating comprising at least one
barrier material,
and an outer coating comprising at least an anti-foaming agent, wherein the
granule has at
least 10% less dust as measured by a Heubach test than a granule without the
antifoaming
agent prepared by a similar process.
Another embodiment is a method of producing the above granules. The granules
are produced by preparing a mixture of compounds, including an allergenic
component to be
incorporated into a granule; adding an antifoam agent to the mixture; and
using the mixture
comprising the antifoam to form a granule or a layer thereof. In another
embodiment of
producing the granules, the antifoam agent is mixed with the allergenic
component. In yet
another embodiment of the method, the antifoam agent also is mixed with a
barrier layer
which surrounds the allergenic component. In yet another embodiment of the
method, the
antifoam agent is added only to a coating that surrounds a barrier layer over
the allergenic
component.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a granule with decreased dust production. The
granule is produced by a process that includes the addition of an antifoaming
agent. The
invention includes any process in which antifoam is added such that a
resultant granule
produces decreased dust as compared with a granule prepared in a process
without
antifoam added.
As pointed out above, a critical issue in the use of enzymes in many consumer
or
industrial applications arises from the fact that enzymes are often potential
allergens.
Accordingly, a need exists for enzyme granules to be formulated so as to
minimize the risk
of sensitization and allergic reaction on the part of factory workers who are
exposed to
enzymes as raw materials, for example in laundry detergent manufacturing
factories, and
also on the part of the general public which may be exposed to enzyme
containing granules
in consumer products. Manufacturing operations such as conveying, sieving,
blending, and
filling can exert attritional forces on enzyme granules which have a tendency
to cause
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breakage of granules and liberation of enzymes which can then form airborne
dusts or
aerosols. Significant efforts involving various granulation and encapsulation
technologies
have been directed towards minimizing the potential of enzyme granules to form
such
allergenic dusts. For example, U.S. Patent No. 4,106,991 (Markussen) describes
the use of
cellulose fibers and binders in a drum granulator to produce a tougher, more
attrition
resistant granule. Similarly, PCT Publication No. WO 93/07263 (Genencor)
describes a
process for making a superior low dust granule in a fluidized bed spray-
coater, comprising a
core, an enzyme layer and an outer coating layer, by utilizing polyvinyl
alcohol as a binder
and coating agent.
As used herein, the term "dust" refers to the tendency of a granule, upon
degradation
or breaking of the granule structure, to liberate fine airborne particulates.
Granule dust is
routinely measured in the industry. For example, granule dust can be measured
by several
different techniques, each technique being well suited for specific conditions
and not
necessarily being interchangeable. However, two techniques in common use
within the
enzyme industry have been validated for their ability to predict the actual
tendency of
mechanically weaker granules to release higher levels of enzyme into the air
in detergent
manufacturing plants.
Two enzyme dust test methods which provide excellent predictive results
include the
Elutriation Test and the Heubach Attrition Test. Each of these tests is well
known in the
industry. However, for the convenience of the reader, the tests are briefly
summarized as
follows. In the Elutriation Test, 60 grams of enzyme granules are place on a
porous glass
frit at the bottom of a tall glass tube and fluidized with a constant dry
airstream at 0.8 m/s for
a period of 20 to,40 minutes. In the Heubach Attrition Test, 13.5 grams of
granules are
placed in a small, cylindrical chamber fitted with a rotating paddle and four
stainless steel
balls, which rotate while dust particles are stripped from the moving bed of
granules by an
airstream for 20 minutes. In both methods, the dust particles stripped off by
the airstream
are deposited on an external filter pad, which is subsequently assayed
gravimetrically for its
total weight ("total dust") or assayed biochemically for its active "enzyme
dust". While these
methods have been found useful by the Applicants, one of skill in the art will
recognize that
suitable methods of dust determination include any reliable method for
reproducibly
subjecting enzyme granules to forces which result in granule breakage or
attrition.
Preferably, the granule of the invention produces at least 20% less dust, more
preferably at least 40% less dust, even more preferably at least 60% less dust
and even
more preferably at least 80% less dust, and most preferably at least 90% less
dust than a
comparable granule made according to an identical process but for the lack of
added
antifoam being present in the resulting granule.
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As used herein, "antifoam" or "antifoam agent" means compounds routinely used
to
prevent or break foam in industrial applications. These can also be referred
to as
defoamers, or defoaming agents. These compounds are surface active substances
which
decrease the surface elasticity of liquids and prevent metastable foam
formation. The foam
breaks as a result of the tendency to attain the equilibrium between the
surface elasticity of
the liquid and the surface active substances. (Vardar-Sukan, Recent Adv.
Biotechnol.
(1991), pp. 113-146). A number of compounds find application as antifoam
agents,
including fats, oils, waxes, aliphatic acids or esters, alcohols, sulfates,
sulfonates, fatty
acids, soaps, nitrogenous compounds, phosphates, polyglycols, sulfides, thio
compounds,
siloxanes and halagenated and inorganic compounds (Ghildyal, Adv. Appl.
Microbiol.
(1988), vol. 33, pp. 173-222). Preferably, the antifoam used is consistent
with use in a
bioprocess. Particularly, oils, fatty acids, esters, polyglycols and siloxanes
are useful. Most
preferably, the inventors herein have determined that an excellent antifoam
agent is
ethylene oxide propylene oxide co-polymer. An example of an ethylene-oxide
propylene-
oxide co-polymer having an approximate molecular weight of 2200 is MazuTM,
available
commercially from Mazer Chemicals, Inc.
According to a preferred embodiment of the invention, the amount of antifoam
added
is sufficient to significantly reduce the dust potential of the resulting
granule. Preferably, the
antifoam is added in a quantity which results in a weight percentage in the
final granule
equal to between about 0.25% and 10% w/w; more preferably between 0.35% and 5%
w/w
and most preferably between 0.5% and 2% w/w.
The antifoam agent may be added during any step of the process towards the
production of a granule. Accordingly, the antifoam may be added to the enzyme
fermentation broth, during a step involving recovery or purification of
enzyme, as a
constituent in any formula related to the granule or a layer of a granule. As
one of skill in the
art will readily recognize, antifoam agent can be added at numerous different
steps of the
granule production process, the best method depending on the specific granule
production
process. Thus, the present invention is not intended to be limited to any
specific type of
granule or granule production method but is capable of numerous modifications
or variations
of the methods described below.
In a preferred embodiment of the invention, the granule is a layered granule
in which
different layers comprise different constituents intended for a various
benefits or effects. In
a typical layered granule, as described in more detail below, it is possible
to include any of a
number of layers. For example, the seed or core may be coated with any
combination of
bleach layers, barrier layers, coating layers, enzyme or other protein layers
and other
protective or active layers.
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In one embodiment, the composition of the invention is formed by the
production of a
particulate, or core, about a small seed or carrier particle. A seed or
carrier particle is an
inert particle upon which a further material (along with a binder and,
optionally, one or more
proteins such as enzymes) can be deposited (e.g., coated, layered, etc.).
Suitable seed
s materials include inorganic salts, sugars, sugar alcohols, small organic
molecules such as
organic acids or salts, minerals such as clays or silicates or a combination
of two or more of
these. Suitable soluble ingredients for incorporation into seed particles
include sodium
chloride, potassium chloride, ammonium sulfate, sodium sulfate, sodium
sesquicarbonate,
urea, citric acid, citrate, sorbitol, mannitol, oleate, sucrose, lactose and
the like. Soluble
ingredients can be combined with dispersible ingredients such as talc, kaolin
or bentonite.
Seed particles can be fabricated by a variety of granulation techniques
including:
crystallization, precipitation, pan-coating, fluid-bed coating, fluid-bed
agglomeration, rotary
atomization, extrusion, prilling, spheronization, drum granulation and/or high
shear
agglomeration. In the particulates of the present invention, if a seed
particle is used, then
the ratio of seed particles to particulates is 1:1 to 1:4 wt/wt. Similarly, in
the granules of the
present invention, the ratio of cores to granules also is 1:1 to 1:4 wt/wt.
Preferably, the seed
particle delivers acceptable strength while not adversely affecting the
density of the final
core or granule.
Suitable binders, contemplated for use herein, include common yellow dent
starch,
modified starches (e.g., hydroxypropyl addition, ethoxylation, acetylation,
acid thinning etc.),
sugars (e.g., sucrose, dextrose, fructose, lactose etc.), maltodextrin,
polyvinylpyrolidine
(PVP), polyethylene glycol (PEG), xanthum gum, gum arabic, acacia gum,
alginate,
carageenan, waxes (e.g., carnuba, beeswax, paraffin and blends thereof), high
melting point
surfactants (e.g., mp between 40 and 80 C).
Proteins that are within the scope of the present invention include
pharmaceutically
important proteins such as hormones or other therapeutic proteins and
industrially important
proteins such as enzymes. In a preferred embodiment, any enzyme or combination
of
enzymes may be used in the present invention. Preferred enzymes include those
enzymes
capable of hydrolyzing substrates, e.g. stains. Preferred enzymes known as
hydrolases
may be used and include, but are not limited to, proteases (bacterial, fungal,
acid, neutral or
alkaline), amylases (alpha or beta), lipases, cellulases and mixtures thereof.
Particularly
preferred enzymes are subtilisins and cellulases. Exemplary subtilisins are
described in
U.S. Patent 4,760,025, EP Patent 130 756 131 and PCT Application WO 91/06637.
Exemplary cellulases include Multifect L250Tm and
PuradaxTM, commercially available from Genencor International. Other enzymes
that can be
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used in the present invention include oxidases, transferases, dehydratases,
reductases,
hemicellulases and isomerases.
Among the places in the granule where the enzyme can be loaded include:
centrally
within the core or seed material (e.g., in a layer around a centrally located
seed particle);
intermixed (e.g., homogeneously) with the core or seed material; as a layer
over the core or
seed material, or surrounding, the core or seed material; as a layer separated
from the core
material by one or more other layers; as well as any combination thereof.
Plasticizers may be used to protect or facilitate a particular layer or can be
used to
protect the granule as a whole. Suitable plasticizers useful in the present
invention include
polyols such as glycerol, propylene glycol, polyethylene glycol (e.g., low MW
PEGs), urea,
or other known plasticizers. Suitable anti-agglomeration agents include fine
insoluble or
sparingly soluble materials such as talc, Ti02, clays, amorphous silica,
magnesium stearate,
stearic acid and calcium carbonate. Thus, plasticizers and anti-agglomeration
agents can
be included, for example, in an overcoating applied to a granule.
A barrier layer can be used to slow or prevent the diffusion of substances
that can
adversely affect the protein or enzyme in the granule. The barrier layer can
be made up of a
barrier material and can be coated over the core and/or over an enzyme layer
that
surrounds the core; and/or the barrier material can be included in the core.
Suitable barrier.
materials include, for example, starch, inorganic salts or organic acids or
salts. In one
embodiment, the barrier layer comprises starch and a binder (e.g., sucrose)
coated over an
enzyme-containing core.
As noted above, the granules of the present invention can comprise one or more
coating layers any of which may be produced according to the method of the
invention. For
example, such coating layers may be one or more intermediate coating layers or
such
coating layers may be one or more outside coating layers or a combination
thereof, any of
which may be produced with the addition of an antifoam agent. In addition,
coating layers
may be added and may serve any of a number of functions in a granule
composition,
depending on the end use of the enzyme granule. For example, coatings may
render the
enzyme resistant to oxidation by bleach, prevent enzyme leakage, bring about
the desirable
rates of dissolution upon introduction of the granule into an aqueous medium,
or provide a
barrier against ambient moisture in order to enhance the storage stability of
the enzyme and
reduce the possibility of microbial growth within the granule.
Suitable coatings include water soluble or water dispersible film-forming
polymers
such as polyvinyl alcohol (PVA), polyvinyl pyrrolidone (PVP), cellulose
derivatives such as
methylcellulose (MC), hydroxypropyl methylcellulose (HPMC), hydroxyethyl
cellulose,
carboxymethyl cellulose, hydroxypropyl cellulose, polyethylene glycol,
polyethylene oxide,
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gum arabic, xanthan, carrageenan, chitosan, latex polymers, and enteric
coatings.
Furthermore, coating agents may be used in conjunction with other active
agents of the
same or different categories.
Suitable PVAs for incorporation in the coating layer(s) of the granule include
partially
hydrolyzed, fully hydrolyzed and intermediately hydrolyzed PVAs having low to
high degrees
of viscosity. Preferably, the outer coating layer comprises partially
hydrolyzed PVA having
low viscosity. Other vinyl polymers which may be useful include polyvinyl
acetate and
polyvinyl pyrrolidone. Useful copolymers include, for example, PVA-
methylmethacrylate
copolymer and PVP-PVA copolymer and enteric co-polymers such as those sold
under the
tradename Eudragit (Rhone Poulenc).
The coating layers of the present invention may further comprise one or more
of the
following: plasticizers, extenders, lubricants, pigments, and optionally
additional proteins
such as enzymes. Suitable plasticizers useful in the coating layers of the
present invention
are plasticizers including, for example, polyols such as sugars, sugar
alcohols, or
polyethylene glycols (PEGS), urea,' glycol, propylene glycol or other known
plasticizers such
as triethyl citrate, dibutyl or dimethyl phthalate or water. Suitable pigments
useful in the
coating layers of the present invention include, but are not limited to,
finely divided whiteners
such as titanium dioxide or calcium carbonate or colored pigments and dyes or
a
combination thereof. Preferably such pigments are low residue pigments upon
dissolution.
Suitable extenders include sugars such as sucrose or starch hydrolysates such
as
maltodextrin and corn syrup solids, clays such as kaolin and bentonite and
talc. Suitable
lubricants include nonionic surfactants such as Neodol, tallow alcohols, fatty
acids, fatty acid
salts such as magnesium stearate and fatty acid esters.
Adjunct ingredients may be added to any of the layers of the enzyme containing
granules of the present invention. Adjunct ingredients may include: metallic
salts;
solubilizers; activators; antioxidants; dyes; inhibitors; binders; fragrances;
enzyme protecting
agents/scavengers such as ammonium sulfate, ammonium citrate, urea, guanidine
hydrochloride, guanidine carbonate, guanidine sulfamate, thiourea dioxide,
monoethanolamine, diethanolamine, triethanolamine, amino acids such as
glycine, sodium
glutamate and the like, proteins such as bovine serum albumin, casein and the
like etc.;
surfactants including anionic surfactants, ampholytic surfactants, nonionic
surfactants,
cationic surfactants and long-chain fatty acid salts; builders; alkalis or
inorganic electrolytes;
bleaching agents; bluing agents and fluorescent dyes and whiteners; enzyme
stabilizers
such as betaine, peptides and caking inhibitors.
Preferably, the granules produced in accordance with the present invention are
roughly round, or spherical, in shape.
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The granules described herein may be made by methods known to those skilled in
the art of particle generation, including but not limited to marumerization,
drum granulation,
fluid-bed spray-coating, pan-coating, or other suitable process, or
combinations of such
techniques. Several exemplary methods for producing the particulate
compositions and
s granules of the invention are described next.
In one preferred embodiment of fluid bed spray coating, a seed particle is
charged
into a fluid bed coater and fluidized. A coating solution consisting of a
binder or binder
system along with a non-porous or minimally porous, low-density material
(e.g.,
hollowspheres) and optionally including other low-density materials is sprayed
onto the seed
to generate a particulate or core. Also, the non-porous or minimally porous,
low-density
material (and other low-density materials, if applicable) may be added dry
along with
application of a binder spray in either a pan or fluidized bed coater. After
the core is
generated, an enzyme can be layered onto the core. Optionally, this may be
followed by
other layers whose purpose can be, for example, buffering, providing a
protective barrier,
bulking, providing another value/performance added material. Finally, a
cosmetic coating
can be applied to provide aesthetics and protection from the environment. If
desired, the
entire process can be performed in a pan coater. Moreover, any part of this
process can be
performed in either a pan coater or a fluidized bed coater.
Suitable seed particles for use in the just-described method include, for
example, a
sugar crystal, salt crystal, non-pareil, a prill with an acceptable melting
point, an extruded
particulate, a particulate from a drum granulation, etc.
In another embodiment for forming a granule, a core or seed material can be
blended in a solution consisting of melted components and little or no water
or other solvent.
This solution can be fed to a spinning disc, centrifugal nozzle or any other
type of prilling
device which. is used to generate spherical particles of sizes between 50 and
3000 urn. The
prills are generated at some height above a collection area which allows them
to cool and
harden as they fall. Alternatively, a counter-current chilling air-stream may
be used to
facilitate prill hardening and control particle velocities. Optionally, enzyme
may be added to
the hot-melt solution in the form of a dry powder, enzyme-crystal slurry or
paste, enzyme
precipitate slurry or paste or in a solubilized form in either an aqueous or
non-aqueous
solvent. In any of the above enzyme additions, solvent of liquid carrier
concentration in the
hot-melt cannot rise to above a level where spheroidal, non-friable prills are
no longer
formed. These enzyme prills can then be cosmetically coated, as an option.
In a further embodiment, enzyme granules of the present invention are made by
an
extrusion method by adding the core material to the dry blend and then
processing as
described in, for example, U.S. Patent No. 5,739,091
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In yet another embodiment, low-density enzyme granules of the present
invention
are made by a drum granulation method by adding the core material to the dry
blend and
processing as described in, for example, in PCT WO 90/09440
In still a further embodiment, the core material can be blended into a
solution/slurry
that is used to produce the core of a microencapsulated product. This solution
can be
sprayed along with a shell solution through a binary phase nozzle, where the
core solution
exits through the inner liquid port and the shell solution exits through the
outer concentric
liquid port, and atomized via centrifugal force, mechanical vibration, jet
cutting, sonics, cross
shear from a liquid or gas stream, electromagnetic field, etc. Depending on
the shell, the
microencapsulate can be collected in a liquid based collection bath, a solid
media that
facilitates free-flow of the product or in static or countercurrent air stream
that allows
hardening/setting up of the product before it reaches a collection vessel.
Optionally, the
microencapsulate can be dried and/or cosmetically coated.
The shell can be composed of any material(s) that efficiently entrap the inner
core
and provide enough rigidity so that the microcapsule can be handled in
relevant applications
without significantly deforming, agglomerating, decomposing or in other ways
becoming
non-utile.
The granules described herein may be made by methods known to those skilled in
the art of enzyme granulation, including pan-coating, fluid-bed coating, fluid-
bed
agglomeration, grilling, disc granulation, marumerization, spray drying,
extrusion, centrifugal
extrusion, spheronization, drum granulation, high shear agglomeration, or
combinations of
these techniques.
The following examples are representative and not intended to be limiting. One
skilled in the art could choose other proteins, protein cores, enzymes, enzyme
cores, seed
particles, methods and coating agents based on the teachings herein.
Examples
Example 1
ao In this example, a granule comprising.a seed and three layers was produced
wherein
antifoaming agent was added to the enzyme layer. A control was prepared with
no antifoam
added and the dust levels were compared. To produce the granules, 1.0 kg of
sucrose
crystals was sieved to between 35 and 50 mesh were charged into Glatt 3 fluid
bed coater
and fluidizer. 1.6 Kg of an aqueous protease solution with 15.5% total dry
solids was added
to 3.27 kg of an aqueous solution containing 0.84 kg of sucrose and 0.84 kg of
cornstarch.
Lot #2 differed from lot #1 by the addition of 47 grams of the antifoaming
agent ethylene
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oxide propylene oxide co-polymer (MazuTM DF204) to the above described
formulation. The
protease solution was sprayed onto the sucrose seed crystal under the
following conditions:
Fluid feed rate 43 gram/min
s Atomization pressure 20 PSI
Product temp. 45 C
Inlet air flow 100 CFM
The coated particles were then coated with an aqueous solution containing 1.6
kg
,o (50% w/w) of magnesium sulfate heptahydrate. This coating was applied under
the
following conditions:
Fluid feed rate 50 gram/min
Atomization pressure 30 PSI
15 Product temp. 45 C
Inlet air flow 100 CFM
The magnesium sulfate coated particles were then cosmetically coated with 3.5
kg of
an aqueous solution containing 267g (6% w/w) titanium dioxide, 111 g (2.5%
w/w)
20 methylcellulose (Methocell, available from the Dow Company), 111 g (2.5%)
Purecote B790
(available from Grain Products Corp), 67 g (1.5% w/w) neodol 23/6.5, and 74 g
(1.7%w/w) of
polyethylene glycol at a MW of 600. The cosmetic coating was applied under the
following
conditions:
25 Fluid feed rate 43 gram/min
Atomization pressure 40 PSI
Product temp. 45 C
Inlet air flow 100 CFM
30 The results show that adding antifoaming agent to the enzyme layer of the
granule
= reduces the dust levels in both the Heubach and Elutriation tests.
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LOT #1 LOT #2
Seed: Seed:
25% sucrose 25% sucrose
Enzyme Laver Enzyme Laver
17.8% Corn Starch 17.8% Corn Starch
17.8% sucrose 17.8% sucrose
5.2% UF conc. Solids 5.2% UF conc. Solids
1 % antifoam
2nd Laver 2nd Laver
20% MgSO4.7H20 20% MgS04.7H20
3rd Laver 3rd Laver
2.5% Purecote 790 2.5% Purecote 790
2.5% Methyl cellulose A15 2.5% Methyl cellulose A15
1.5% Neodol 1.5% Neodol
1.7% PEG 600 1.7% PEG 600
6.0% Ti02 6.0% Ti02
Elutriation
Heubach Dust
TEST RESULTS mg/pad GU/60g
Lot #1 7.8 1.2 (0.014gg/60g)
Lot #2 1.7 0.23 (0.0026 k9/60g)
Example 2
In this experiment, antifoaming agent was added to the first layer (comprising
enzyme) and the second layer (a coating layer comprising corn starch, titanium
dioxide and
neodol) and the dust potential was compared to a granule made without
antifoam.
Lot 1 was prepared as follows:
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25 kg sucrose crystals sieved to between 35 and 50 mesh were charged into
TM
Deseret 60 fluid bed coater and fluidizer. 39 Kg of an aqueous protease
solution with
15.5% total dry solids was added to 63 kg of an aqueous solution containing
22.5 kg of
sucrose and 22.5 kg of cornstarch.
= 5
Lot 2 was prepared as follows:
25 kg sucrose crystals sieved to between 35 and 50 mesh were charged into
TM
Deseret 60 fluid bed coater and fluidizer. 39 Kg of an aqueous protease
solution with
15.5% total dry solids was added to 63 kg of an aqueous solution containing
21.3 kg of
sucrose and 21.3 kg of cornstarch and 1.2 kg (1 %w/w) of Mazu DF204.
Protease solutions were sprayed onto the sucrose crystals under the following
conditions:
Fluid feed rate 750 gram/min
Atomization pressure 75 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
The coated particles were then coated with an aqueous solution containing 82.4
kg
(40% w/w) of 11.7 kg (10.2% w/w) of sucrose, 11.7 kg of cornstarch, 6.9 kg
(6.0% w/w)
titanium dioxide and 1.5 kg (1.3% w/w) of neodol. Lot #2 had 1.2 kg (11%) mazu
added to
its spray solution. This coating was applied under the following conditions:
Fluid feed rate 1200 gram/min
Atomization pressure 60 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
The coated particles were then cosmetically coated with 65.8 kg of an aqueous
= solution containing 2.94 kg (2.5% w/w) hydroxymethylcellulose E15, and 353 g
(0.3% w/w)
of polyethylene glycol at a MW of 600. The cosmetic coating was applied under
the
following conditions:
Fluid feed rate 750 gram/min
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Atomization pressure 75 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
As shown below, adding Mazu as an antifoam agent to layers 1 and 2 of the
granule
reduces the Heubach total dust levels.
LOT #1 LOT #2
Seed: Seed:
25% sucrose 25% sucrose
Enzyme Layer Enzyme Laver
19.6% Corn Starch 18.6% Corn Starch
19.6% sucrose 18.6% sucrose
5.3% UF conc. Solids 5.3% UF conc. Solids
1 % antifoam
2nd Laver 2nd Laver
10.2% corn starch 10.2% corn starch
10.2% sucrose 10.2% sucrose
1.3% Neodol 1.3% Neodol
6.0% TiO2 6.0% TiO2
1 % antifoam
3rd Laver 3rd Laver
2.5% HPMC E15 2.5% HPMC E15
0.3% PEG 600 0.3% PEG 600
Heubach
TEST mg/pad
RESULTS
Lot #1 8.0
Lot #2 0.1
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Example 3
In this example, antifoam was added to the third layer of a granule and
compared to
a granule prepared with no antifoaming agents.
25 kg sucrose crystals were sieved to between 35 and 50 mesh were charged into
Deseret 60 fluid bed coater and fluidizer. 54 Kg of an aqueous protease
solution with
21.4% total dry solids was added to 73 kg of an aqueous solution containing
20.6 kg of
sucrose and 20.6 kg of cornstarch.
Protease solutions were sprayed onto the sucrose under the following
conditions:
Fluid feed rate 750 gram/min
Atomization pressure 75 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
The coated particles were then coated with an aqueous solution containing 82.4
kg
(40% w/w) of 11.7 kg (10.2% w/w) of sucrose, 11.7 kg of cornstarch, 6.9 kg
(6.0% w/w)
titanium dioxide and 1.5 kg (1.3% w/w) of neodol. This coating was applied
under the
following conditions:
Fluid feed rate 1200 gram/min
Atomization pressure 60 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
Lot 1 coated particles were then cosmetically coated with 65.8 kg of an
aqueous
solution containing 2.94 kg (2.5% w/w) hydroxymethylcellulose E15, and 353 g
(0.3% w/w)
of polyethylene glycol at a MW of 600. Lot #2 had 1.2kg (1 %w/w) Mazu DF204
added to
the spray 3 solution. The cosmetic coating was applied under the following
conditions:
Fluid feed rate 750 gram/min
Atomization pressure 75 PSI
Product temp. 45 C
Inlet air flow 1200 CFM
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As shown below, adding Mazu antifoam to the 3rd layer of the D-type granule
reduces the
Heubach total dust levels.
LOT #1 LOT #2
Seed: Seed:
25% sucrose 25% sucrose
Enzyme Layer Enzyme Layer
18.2% Corn Starch 18.2% Corn Starch
18.2% sucrose 18.2% sucrose
5.3% UF conc. Solids 5.3% UF conc. Solids
2nd Layer 2nd Layer
10.2% corn starch 10.2% corn starch
10.2% sucrose 10.2% sucrose
1.3% Neodol 1.3% Neodol
6.0% Ti02 6.0% Ti02
3rd Layer 3rd Layer
2.5% HPMC E15 2.5% HPMC E15
0.3% PEG 600 0.3% PEG 600.
1.0 % Mazu DF204
Heubach
TEST mg/pad
RESULTS
Lot #1 12.3
Lot #2 1.4
