Title of Invention

"PERFUMING OR FLAVOURING MICROCAPSULES COMPRISING AN EXPLOSION SUPPRESSANT"

Abstract A spray-dried powder of starch microcapsules comprising, as ingredients: a carrier material of a starch; at least one perfuming ingredient present in an amount which is between 15 and 60% by weight of the microcapsules' dry weight; and an explosion suppressant in an amount of 2 to 20% by weight of the microcapsules' dry weight, with the explosion suppressant selected from the group consisting of C1-C12 carboxylic acids, salts of C1-C12 carboxylic acids, and mixtures thereof, with the explosion suppressant present in an amount to provide the powder with an St-1 dust hazard explosive classification, wherein the spray dried powder is obtained by spray drying of an emulsion that includes the ingredients with the explosion suppressant present so that the powder has a reduced tendency to explode when being spray dried from the emulsion.
Full Text

Technical Field
The present invention relates to the field of perfumery and to the flavour industry.
It concerns more particularly perfuming or flavouring microcapsules characterised by the
fact that, when subjected to a sufficiently powerful ignition source, their rapid combustion
reaction is weak or moderate. In fact, the microcapsules of the invention comprise an
effective amount of a explosion suppressant susceptible of reducing the violence of their
explosion, so as to classify these particles in a dust hazard class St-1.
Background of the Invention and Problems to be Solved
Microcapsules are employed to a large extent in the perfumery and flavouring
industries. They constitute delivery systems for perfuming or flavouring ingredients and
can be advantageously used in a very large number of applications. The encapsulation of
active substances such as perfuming or flavouring ingredients provides at the same time a
protection of the ingredients there-encapsulated against "aggressions" such as oxidation or
moisture and allows, on the other hand, a certain control of the kinetics of flavour or
fragrance release to induce sensory effects through sequential release.
Now, the numerous advantageous properties of microcapsules in these fields are
opposed to other properties that must be taken into account during their preparation,
transportation, storage and handling. In fact, such delivery systems, due to their nature,
and in particular to the fact that they encapsulate volatile and flammable substances,
constitute combustible dusts which can, when dispersed in air or another oxygen-
containing gas, form readily ignitable mixtures. When ignited by a sufficient powerful
ignition source, the result is a rapid combustion reaction with advancing pressure and
flame front.
This issue becomes important during the preparation of microcapsules. In
particular, spray-drying and fluidised-bed encapsulation processes are highly concerned
by this issue, as they are both based on the use of an equipment wherein particles are
suspended in hot air as fine particles and can therefore undergo explosion during their
preparation.

Spray-drying is the most common encapsulation technique used to stabilise
volatile substances such as flavours or fragrances, by encapsulating them in a solid form,
suited to many applications. Spray-dried powders are commonly made in an usual spray-
drying equipment. Spray-drying is usually effected by means of a rotating disc or of
multicomponent nozzles. Detailed techniques are described for instance in K. Masters,
Spray-drying Handbook, Longman Scientific and Technical, 1991.
Fluidised beds are used for spraying a coating on a core material fluidised in a
bed, or agglomerating and/or granulating powders. This encapsulation technique is also
well known and is described for instance in EP 70719 or in US 6,056,949, the contents of
which are hereby included by reference.
Both the above-described encapsulation equipments being susceptible to
explosions of particles suspended in the air, they thus have to be adapted as a function of
the technical safety parameters characterising the particles there-treated. In particular,
they have to be dimensioned as a function of the violence of explosions that can occur
during the preparation of microcapsules. Therefore, the problem of reducing the violence
of possible explosions of powder products resulting from such encapsulation processes is
of paramount importance for the industry.
For the safe handling of combustible substances, it is imperative to know the
dangerous properties of a product. The reliable way to characterise the combustible and
explosive properties of a product is to subject a sample of the product to various tests and
classify the results in accordance with the technical safety characteristics. The
international standards (VDI Guideline 2263 part 1 : Dust Fires and Dust Explosions,
Hazard Assessment - Protective Measures, Test Methods for the Determination of Safety
Characteristics of Dusts, Beuth, Berlin, May 1990) describe the test equipments
(Modified Hartmann apparatus and Close apparatus, 20-litre sphere apparatus) and
methods, namely the ISO standard procedure ISO 6184/1. These methods allow to
determine physical constants such as the maximum explosion behaviour of a combustible
dust in a closed system. A pyrotechnic igniter with a total energy of 10 kJ is used as
ignition source. From test methods described in the mentioned guidelines, a characteristic
constant, KSt, which is dust specific is determined. As there are so many such dusts
produced and processed in industrial practice, for example for pharmaceutical and cereal,
flour products, it is appropriate to assign this maximum explosion constant to one of the
several dust explosion classes and to use these as a basis for the dimensioning of

constructional protective measures. The correspondence between these classes hereafter
referred as dust hazard classes, and the constant K-st is the following :
Dust Hazard Class Product Specific Constant K-st [bar.m.s-1]
St-1 0 to 199
St-2 200 to 299
St-3 > 300
Now, although some perfuming and flavouring ingredients are classified in a dust
hazard class St-1, a large number of these ingredients and thus the microcapsules
encapsulating them, and depending on the volatility of the perfuming or flavouring
ingredients, are still classified under an St-2 dust hazard class and thus require production
equipments specifically adapted to the violence of possible explosions, which of course
can be very costly.
WO 03/043728 A1 (FIRMENICH) discloses perfuming or flavouring
microcapsules having fireproofing agents dispersed in or absorbed within a polymeric
carrier material, whereby these fireproofing agents were basically inorganic salts. In view
of these fireproofing agents, other agents suitable as explosion suppressants having
further beneficial properties are needed. There is in particular a need of finding more
efficient fireproofing agents, which can be used with similar efficiency in smaller
amounts, and there is a need of fireproofing agents that have a beneficial effect on the
hygroscopicity of the perfuming or flavouring microcapsules, notably it would be an
advantage to have a fireproofing agent that reduces hygroscopicity of the perfuming or
flavouring microcapsules if compared to fireproofing agents of the prior art. In addition,
the fireproofing agents disclosed in WO 03/043728 are not always suitable for use in food
applications and other solutions have thus to be found.
Description of the Invention
Remarkably, we have been able to establish that new explosion suppressants being
C1-C12 carboxylic acids, salts of C1-C12 carboxylic acids, and mixtures thereof could be
added directly to perfuming and flavouring microcapsules in an amount effective to
reduce the violence of possible explosions during their preparation, in particular when

suspended in hot air. The K.St constant of microcapsules comprising the new explosion
suppressants could thus be effectively reduced. Very surprisingly, these new explosion
suppressants also reduce the hygroscopicity of powders comprising the microcapsules of
the present invention.
Therefore, in a first aspect, the present invention provides perfuming or flavouring
microcapsule comprising at least one perfuming or flavouring ingredient dispersed in or
adsorbed within a polymeric carrier material, characterised in that the microcapsule
further comprises an effective amount of a explosion suppressant selected from the group
of C1-C12 carboxylic acids, salts of C1-C12 carboxylic acids, and mixtures thereof.
In a second aspect, the present invention provides methods for the preparation of
perfuming or flavouring compositions according to the invention.
In a further aspect, the present invention provides the use of a explosion
suppressant selected from the group consisting of C1-C12 carboxylic acids, salts of C1-C12
carboxylic acids, and mixtures thereof in the composition of a microcapsule for reducing
the violence of the explosion of the microcapsule.
In a still further aspect, the present invention provides a method for reducing
explosivity of a powdered composition, the method comprising the step of
- adding to the powdered composition a fireproof agent selected from the group
consisting of C1-C12 carboxylic acids, salts of C1-C12 carboxylic acids, and mixtures
thereof to the powdered composition, and/or,
- incorporating the fire proof in and/or within particles of the powdered composition,
and/or,
- coating the fire proof agent onto the powdered composition.
Furthermore, the present invention provides perfumed product and a food,
beverage or pharmaceutical product, characterised in that it comprises the flavouring
and/or perfuming microcapsule of the present invention.
As mentioned above, the St-class of a microcapsule is deduced from the value of
its product specific constant K.st (see correspondance Table above). The K.st parameter is
measured by means of the ISO standard procedure ISO 6184/1 in a 201 sphere apparatus.
This equipment and the methods of measurement of K.st are described in International
standards, hereby included by reference (VDI Guideline 2263 part 1 : Dust Fires and Dust
Explosions, Hazard Assessment - Protective Measures, Test Methods for the
Determination of Safety Characteristics of Dusts, Beuth, Berlin, May 1990).

The perfuming or flavouring microcapsules of the invention comprise an effective
amount of a explosion suppressant which is capable of reducing the violence of the
explosion of the microcapsules possibly induced by their suspension in the air during their
preparation. This is very advantageous considering that such delivery systems are mainly
composed of highly volatile ingredients which constitute therefore combustible dusts.
Such volatile ingredients had to be used in the past in limited proportions in compositions
subjected to processes involving the suspension of particles in hot air. Now, the solution
provided by the present invention allows to use higher quantities of these ingredients, and
therefore provides an advantageous alternative to the prior use of precursors of certain
particularly volatile ingredients.
The invention therefore provides an advantageous solution as regards the problem
of the preparation of perfuming and flavouring microcapsules and powder products, in
particular for preparations via processes involving a spray-drier or a fluidised bed,
wherein fine particles are suspended in the air and are therefore more susceptible of
exploding. Under an St-1 class, the violence of the explosion will be a weak or at least
moderate reaction, whereas it would be a strong reaction for a dust hazard class St-2, and
a very strong reaction for a dust hazard class St-3. As a consequence, the equipment used
for the preparation of microcapsules according to the present invention can be
dimensioned accordingly i.e. as St-1 and thus become less costly, whilst guarantying the
same or better manufacture safety conditions.
The term C1-C12 carboxylic acids refers to carboxylic acids that have 1 to
12 carbon atoms, including the C-atom of the carboxyl group. Therefore, if more than one
carboxylic group are present in the carboxylic acid of the present invention, these further
carboxylic group are, equally, to be counted to the 1 to 12 carbon atoms of the carboxylic
acid used as a explosion suppressant according to the present invention.
Preferably, the carboxylic acids and/or their salts that are used as explosion
suppressants in microcapsules of the present invention are linear, branched, cyclic, and/or
aromatic carboxylic acids and/or their salts. The carboxylic acids may be saturated
hydrocarbons. Alternatively, the carboxylic acids may be unsaturated hydrocarbons.
Examples of cyclic carboxylic acids are lactones, for example ascorbic acid. An
example for an aromatic carboxylic acid is salicylic acid.
Preferably, the carboxylic acids and/or their salts are functionalised hydrocarbon
carboxylic acids and/or their salts.

Preferably, the carboxylic acid comprise less than 7, more preferably less than 5
and most preferably less than 3 carbon atoms covalently bound to 2 hydrogen atoms.
Preferably, the carboxylic acid of the present invention comprises 5 or less carbon
atoms with an oxidation number of (-II) or more negative. More preferably, the
carboxylic acid comprises 3 or less carbon atoms having a oxidation number of (-II) or
more negative.
In an embodiment of the present invention, the carboxylic acids and/or their salts
are hydroxy- and/or ceto-functionalised hydrocarbon carboxylic acids and/or their salts.
Preferably, the carboxylic acid of the present invention comprises at least 1 hydroxy
group. Preferably, it comprises at least 2 hydroxy groups.
In a further embodiment of the microcapsules of the present invention, the
carboxylic acids and/or their salts are di-, tri-, or multi carboxylic acids and/or their salts.
Examples of multi carboxylic acids include citric acid, which is C6-tricarboxylic acid.
Preferably, the carboxylic acid is at least a di carboxylic acid. More preferably, it
is at least a tri carboxylic acid, meaning that it carries at least three carboxylic groups.
Preferably, the carboxylic acid and/or their salt is a C4-C8 carboxylic acid and/or
their salt.
In a preferred embodiment of the present invention, the carboxylic acid and/or
their salts are selected from C2-C6 carboxylic acids and/or their salts.
In an embodiment of the perfuming or flavouring microcapsule of the present
invention, the carboxylic acid and/or its salt is selected from the group consisting of acetic
acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic acid, citric acid,
succinic acid, hydroxysuccinic acid, maleic acid, fumaric acid, oxylic acid, glyoxylic
acid, adipic acid, lactic acid, lactic acid, tartric acid, salicylic acid, ascorbic acidthe
potassium, calcium and/or sodium salts of any of the fore-mentioned acid, and mixtures
of any of these.
Preferably, the salts of the carboxylic acids are potassium and/or sodium salts.
More preferably, it is the tripotassium and/or trisodium salt of a tricarboxylic acid. Most
preferably, it is the tripotassium and/or trisodium salt of citric acid.
The above acids and their salts are commercially available and their synthesis, or
isolation from raw materials, is known to the skilled person.

In an embodiment of the present invention, the microcapsule comprises from 0.5
to 80% by weight of explosion suppressant relative to the dry weight of the microcapsule.
Preferably, the microcapsule comprises 1 to 40%, more preferably 2 to 20%), and most
preferably 2 to 10% by weight of explosion suppressant relative to the dry weight of the
microcapsule.
The microcapsule of the invention is based on the presence of at least one
perfuming or flavouring material and a polymeric carrier material.
The perfuming or flavouring ingredient, in the form of one sole ingredient or in
the form of a composition, either in isolation or, optionally, in a solution or suspension in
solvents and adjuvants of current use, represents from 1 to 70%, and preferably from 15
to 60%, most preferably 20 to 45% by weight relative to the total weight of the
microcapsule.
The terms perfume or flavour ingredient or composition as used herein are
deemed to define a variety of fragrance and flavour materials of both natural and
synthetic origins. They include single compounds and mixtures. Specific examples of
such components may be found in the current literature, e.g. in Perfume and Flavour
Chemicals by S. Arctander, Montclair, N.J. (USA); Fenaroli's Handbook of Flavour
Ingredients, CRC Press or Synthetic Food Adjuncts by M.B. Jacobs, van Nostrand Co.
Inc., and other similar text books ; and are well-known to the person skilled in the art of
perfuming, flavouring and/or aromatising consumer products, i.e. of imparting an odour
or a taste to a consumer product.
According to the present invention, the perfume or flavour ingredient or
composition is dispersed in, coated onto or absorbed in a carrier material.
Preferably, the carrier material comprises carbohydrates. For example, the carrier
material comprise mono-, oligo- and/or polysaccharides, wherein the prefixes oligo- and
poly are as defined below.
In an embodiment of the present invention, the carrier material comprises a
monomelic, oligomeric or polymeric carrier material, or mixtures of two or more of these.
An oligomeric carrier is a carrier wherein 2-10 monomeric units are linked by covalent
bonds. For example, if the oligomeric carrier is a carbohydrate, the oligomeric carrier
may be sucrose, lactose, raffinose, maltose, trehalose, fructo-oligosaccharides, to name a
few examples only.

Examples of a monomelic carrier materials are glucose, fructose, mannose,
galactose, arabinose, fucose, sorbitol, mannitol, for example.
Polymeric carriers have more than 10 monomeric units that are linked by covalent
bonds. Non limiting examples of the latter include polyvinyl acetate, polyvinyl alcohol,
dextrines, maltodextrines, natural or modified starch, vegetable gums, pectins, xanthanes,
alginates, carragenans or yet cellulose derivatives such as for example carboxymethyl
cellulose, methylcellulose or hydroxyethylcellulose, and generally all materials currently
used for encapsulation of volatile substances. Preferably, the polymeric carrier comprises
maltodextrin. Most preferably it comprises maltodextrin and modified starch, such as, for
example, alkenyl-succinated starch.
In another embodiment, the perfume or flavour ingredient or composition is
adsorbed within a polymeric carrier material. As non limiting examples of the latter, one
can cite amorphous silica, precipitated silica, fumed silica and aluminosilicates such as
zeolite and alumina.
According to an aspect, the present invention provides methods for the preparation
of perfuming and flavouring microcapsules comprising a explosion suppressant. There are
several alternatives to the method for the preparation of the microcapsules of the
invention. In a first embodiment, the explosion suppressant is added to an aqueous
emulsion consisting of the perfuming or flavouring ingredient or composition dispersed in
the polymeric carrier material. The obtained emulsion is then spray-dried in order to form
a powder. Optionally, an emulsifier may be added to the initial emulsion. This
encapsulation technique does not require a more detailed description herein, as it relies on
conventional spray-drying techniques, which are perfectly well documented in the prior
art [see for example Spray-Drying Handbook, 3rd ed., K. Masters ; John Wiley (1979)]
and currently applied in the food industry or in the flavour and perfume industries.
In another embodiment, the explosion suppressant, in the form of a solid powder,
is simply blended with a spray-dried powder formed from the aqueous emulsion of
perfuming or flavouring ingredient or composition in the polymeric carrier material and
the emulsifier.
A third alternative for the preparation of the microcapsules of the invention
presenting an explosion reaction of reduced violence, is to firstly adsorb the perfuming or
flavouring ingredient or composition within a porous polymeric carrier material as
described above and to further coat the resulting system with a explosion suppressant.

This method of preparation can be carried out in a fluidised bed apparatus, according to
conventional techniques such as those described for instance in EP 70719 or in
US 6,056,949 the contents of which are hereby included by reference. The particles
formed by adsorption of a fragrance or flavour ingredient or composition within the
carrier can thus be coated after granulation, e.g. by spraying a solution, emulsion or melt
of the explosion suppressant, which forms a protective film around the core.
During the granulation process, there can also be used usual additives such as
artificial sweeteners, food dyes, vitamins, antioxidants, anti-foam agents, carbonic acid
generators, or additional flavorants etc. which can be added to the core material or to the
spray emulsion.
The microcapsules of the invention have an average diameter varying from
usually 5 to 800 µm, more preferably 50 to 300 µm.
In an aspect, the present invention provides a method for reducing violence of
explosion of a powdered composition. The composition is preferably a perfuming or
flavouring composition. More preferably, it is a composition comprising flavouring
perfuming and/or perfuming microcapsules. Violence of explosion is determined by the
K.st constant described above. The adding of the explosion suppressant to a powdered
composition may be performed by adding to a spray-dried powdered. However, any way
of dry- or wet-adding the explosion suppressant to a powdered composition is
encompassed. For example, the adding is a dry-blending or dry-mixing with the
components of the powdered composition. Alternatively, the explosion suppressant may
be incorporated in and/or within the particles of a powdered composition. This step may
be performed by adding the explosion suppressant to an aqueous emulsion dispersed in a
polymeric carrier material as described above, followed by drying the obtained emulsion,
for example by spray drying.
In a further alternative, the explosion suppressant may simply be coated onto a powdered
composition. The coating may be performed by coating onto a porous polymeric carrier
material, for example with a fluidised bed apparatus, as discussed above, for example.
The microcapsules of the invention can advantageously be used to impart,
improve, enhance or modify the organoleptic properties of a great variety of edible or
perfumed end products. In the field of perfumery, the perfuming microcapsules resulting
from any embodiment of the process according to the invention can be incorporated in a
perfuming composition such as a perfume, a Cologne or an after-shave lotion, or yet they

can be added to functional products such as detergents or fabric softeners, soaps, bath or
shower gels, deodorants, body lotions, shampoos and other hair-care products, household
cleansers, cleaning and deodorising blocks for toilet tanks. On the other hand, in the case
of flavours encapsulated, the consumer products susceptible of being flavoured by the
microcapsules of the invention may include foods, beverages, pharmaceuticals and the
like.
The concentrations in which the microcapsules of the invention can be
incorporated in such consumer products vary in a wide range of values, which are
dependent on the nature of the product to be perfumed or flavoured. Typical
concentrations, to be taken strictly by way of example, are comprised in a range of values
as wide as from a few ppm up to 5 or 10% of the weight of the flavouring or perfuming
composition or finished consumer product into which they are included.
The invention will be now illustrated but not limited by way of the following
examples wherein temperatures are given in degrees centigrade and abbreviations have
the meaning common in the art.
Embodiments of the Invention
Examples 1-9
Spray-drying of a perfuming emulsions comprising a explosion suppressant
Nine perfuming emulsions were prepared based on different compositions given
in Table 1 below (parts by weight). The compositions are based on two different
perfuming compositions (perfume A and perfume B), whereby different explosion
suppressants were compared:
Example Explosion suppressant
1 and 2 Na3 citrate
3 and 4 Citric acid
5 and 6 K3 citrate
7 and 8 NaH2PO4 (prior art)
9 none (control)

In Examples 1- 9 given in Table 1, stabilizers were first dissolved in the perfume.
The remaining ingredients were homogenised with an equivalent amount of water and
then the perfume was emulsified in this dispersion by means of a Silverstone type fast
stirrer. The mixtures were then spray dried in a Sodeva apparatus with an emulsion output
of 2 kg/h, drying air: 320 m3/h at 350°C and 0.45xl05 Pa.
There were thus obtained 9 fine powders comprising microcapsules, the diameter
of the microcapsules being comprised between 10 and 100µm and the content of liquid
perfume being 36-40% by weight.
The explosive character of the powders was measured with a 20 1 sphere apparatus
(see VDI Guideline 2263 part 1 : Dust Fires and Dust Explosions, Hazard Assessment -
Protective Measures, Test Methods for the Determination of Safety Characteristics of
Dusts, ISO standard procedure ISO 6184/1, Beuth, Berlin, May 1990), and the powders
were attributed dust hazard classes St-1 (Examples 1-8, comprising fireproof agents),
and St- 2-3 (Example 9, no fireproof agent), see details in Table 1.
From Table 1 it can be seen that citric acid, sodium and potassium citrate
effectively reduced explosive violence of the microcapsules. The most effective explosion
suppressant was potassium citrate, which was added at 5% of the composition and which
reduced explosivity to 119 Kst (perfume B) and 132 Kst (perfume A), respectively.
Potassium citrate had thus the same, or even better reducing effect on violence of
explosion than the explosion suppressant of the prior art (WO 03/043728), mono-sodium
phosphate, which was used at much higher concentrations (15wt.-%, Example 9).
In conclusion, the new explosion suppressants of the present invention can reduce
the violence of explosion of perfuming microcapsules and are effective at substantially
lower concentration than explosion suppressant used in similar compositions from the
prior art.



Example 10
Hygroscopy of new explosion suppressants in comparison with the prior art
Hygroscopicity (the tendency to absorb water) of the microcapsules of Examples 5
(present invention) and 7 (prior art) is determined in a Dynamic Vapor Sorption,
commercialised by Surface Measurements Systems Ltd, 3 Warple Mews, Warple Way,
London, W3 ORF, at increasing relative humidity (40%, 50%, 60%, 70%, 80%) to
determine the "melting" point of the two powders at 30°C. The "melting point", in the
context of the present Example 10, refers to the relative humidity at which a powder has
absorbed so much water that it loses its powdery aspect and starts to flow like a liquid,
that is, it "melts". The specific relative humidity at which this happens can be determined
due to the observation of the powder during the water-absorption from humid air by aid of
a camera.
The perfuming microcapsules of Example 5, comprising 5% of potassium citrate
"melts" at a relative humidity of 80% RH, while the perfuming powder of Example 7
(prior art) already "melts" at 60% RH. In additional test, a powdered perfuming
composition comprising 15% potassium citrate was prepared, which was found to "melt"
at 70% RH.
The difference in hygroscopicity in powders comprising microcapsules of the
present invention can be attributed, without being bound by theory, first to the fact that
potassium citrate leads to less hygroscopicity powders than sodium phosphate. In
addition, less of the explosion suppressant needs to be used, which further reduces
hygroscopicity of the powder. In conclusion, the present invention surprisingly provides
powdered perfuming compositions that withstand very humid environments of up to 80%
RH at 30°C.
Example 11
Based on the composition of the perfuming microcapsules given below,
microcapsules are prepared by dry blending a spray dried powder comprising polymeric
carrier and a perfuming ingredient with a explosion suppressant in a powdered form.

Dry blending with explosion suppressant
An emulsion of the following composition was spray-dried in a spray-drier Biichi
(origin : Switzerland) :
Ingredients grams
. Water 150.0
Capsul®1) 67.0
Perfume concentrate2) 33.0
Total 250.0
1) dextrin dioctenylsuccinate ; origin : National Starch, USA
2) origin : Firmenich SA, Geneva, Switzerland
The theoretical yield after evaporation of water is of 100 g of powder containing
33% of perfume.
The explosive character of the powder is measured with a 201 sphere apparatus
(see Examples 1-9), and the powder was attributed a dust hazard class St-2.
The same powder is then mixed with potassium citrate (K3 citrate x 1H2O) in a
powder form, in a ratio of 85:15.
The analysis of the explosive character of the homogeneous mixture, made under
the same condition demonstrated that the mixture is classified as St-1.


WE CLAIM :
1. A spray-dried powder of starch microcapsules comprising, as ingredients:
a carrier material of a starch;
at least one perfuming ingredient present in an amount which is between 15 and 60% by
weight of the microcapsules' dry weight; and
an explosion suppressant in an amount of 2 to 20% by weight of the microcapsules' dry
weight, with the explosion suppressant selected from the group consisting of C1-C12 carboxylic acids,
salts of C1-C12 carboxylic acids, and mixtures thereof, with the explosion suppressant present in an
amount to provide the powder with an St-1 dust hazard explosive classification,
wherein the spray dried powder is obtained by spray drying of an emulsion that includes
the ingredients with the explosion suppressant present so that the powder has a reduced tendency to
explode when being spray dried from the emulsion.
2. The microcapsules as claimed in claim 1, wherein the carboxylic acids or their salts are
hydroxy- or ceto-functionalized hydrocarbon carboxylic acids or their salts.
3. The microcapsules as claimed in claim 1, wherein the carboxylic acids or their salts are
di-, tri-, or multi carboxylic acids or their salts.
4. The microcapsules as claimed in claim 1, wherein the carboxylic acid and/or their salts
are selected from C2-C6 carboxylic acids or their salts.
5. The microcapsules as claimed in claim 1, wherein the carboxylic acid is selected from
the group consisting of acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic
acid, citric acid, succinic acid, hydroxysuccinic acid, maleic acid, fumaric acid, oxylic acid, glyoxylic
acid, adipic acid, lactic acid, tartric acid, salicylic acid, ascorbic acid, the potassium, calcium or sodium
salts of any of the afore-mentioned acids, and mixtures of any of these.
6. The microcapsules as claimed in claim 1, wherein the carboxylic acid is selected from
the group consisting of acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic

acid, succinic acid, hydroxysuccinic acid, maleic acid, fumaric acid, oxylic acid, glyoxylic acid, adipic
acid, lactic acid, tartric acid, salicylic acid, ascorbic acid the potassium, calcium or sodium salts of any
of the afore-mentioned acids, and mixtures of any of these.
7. The microcapsules as claimed in claim 1, wherein the explosion suppressant is
potassium citrate.
8. The microcapsules as claimed in claim 1, wherein the carrier material comprises
maltodextrin.
9. The microcapsules of claim 1, wherein the explosion suppressant is present in an amount
of from 2 to 10% by weight relative to the dry weight of the microcapsules.
10. The microcapsules as claimed in claim 1, wherein the perfume ingredient is present in an
amount of from 20 to 45% by weight relative to the total weight of the microcapsules.
11. A method for reducing violence of explosion of perfuming microcapsules as claimed in
claim 1, which comprises preparing the microcapsules by incorporating the explosion suppressant in or
within the microcapsules.
12. A perfumed product selected from the group consisting of a perfume, a Cologne, an
after-shave lotion, a soap, a bath or shower gel, a deodorant, a body lotion, a shampoo or another hair-
care product, a detergent, a fabric softener, a household cleaner and a cleaning and deodorizing block
for toilet tanks, characterized in that it comprises perfuming microcapsules as claimed in claim 1.
13. A food, beverage or pharmaceutical product, which comprises perfuming microcapsules
as claimed in claim 1.




PERFUMING OR FLAVOURING MICROCAPSULES COMPRISING AN EXPLOSION
SUPPRESSANT
A spray-dried powder of starch microcapsules comprising, as ingredients: a carrier material of a starch;
at least one perfuming ingredient present in an amount which is between 15 and 60% by weight of the
microcapsules' dry weight; and an explosion suppressant in an amount of 2 to 20% by weight of the
microcapsules' dry weight, with the explosion suppressant selected from the group consisting of C1-C12
carboxylic acids, salts of C1-C12 carboxylic acids, and mixtures thereof, with the explosion suppressant
present in an amount to provide the powder with an St-1 dust hazard explosive classification, wherein
the spray dried powder is obtained by spray drying of an emulsion that includes the ingredients with the
explosion suppressant present so that the powder has a reduced tendency to explode when being spray
dried from the emulsion.

Documents:

00855-kolnp-2007 correspondence-1.1.pdf

00855-kolnp-2007 form-3-1.1.pdf

00855-kolnp-2007- correspondence-1.2.pdf

00855-kolnp-2007-assignment-1.1.pdf

0855-kolnp-2007-abstract.pdf

0855-kolnp-2007-assignment.pdf

0855-kolnp-2007-claims.pdf

0855-kolnp-2007-correspondence others.pdf

0855-kolnp-2007-description (complete).pdf

0855-kolnp-2007-form1.pdf

0855-kolnp-2007-form3.pdf

0855-kolnp-2007-form5.pdf

0855-kolnp-2007-international publication.pdf

0855-kolnp-2007-international search authority report.pdf

0855-kolnp-2007-pct others.pdf

0855-kolnp-2007-priority document.pdf

855-KOLNP-2007-(13-01-2012)-CORRESPONDENCE.pdf

855-KOLNP-2007-(13-01-2012)-FORM 3.pdf

855-KOLNP-2007-(17-02-2012)-CORRESPONDENCE.pdf

855-kolnp-2007-abstract.pdf

855-kolnp-2007-amanded claims.pdf

855-kolnp-2007-amanded pages of specification.pdf

855-KOLNP-2007-ASSIGNMENT.pdf

855-KOLNP-2007-CANCELLED PAGES.pdf

855-kolnp-2007-correspondence.pdf

855-kolnp-2007-description (complete).pdf

855-KOLNP-2007-EXAMINATION REPORT.pdf

855-kolnp-2007-form 1.pdf

855-kolnp-2007-form 18.pdf

855-kolnp-2007-form 2.pdf

855-kolnp-2007-form 3.pdf

855-KOLNP-2007-GPA.pdf

855-KOLNP-2007-GRANTED-ABSTRACT.pdf

855-KOLNP-2007-GRANTED-CLAIMS.pdf

855-KOLNP-2007-GRANTED-DESCRIPTION (COMPLETE).pdf

855-KOLNP-2007-GRANTED-FORM 1.pdf

855-KOLNP-2007-GRANTED-FORM 2.pdf

855-KOLNP-2007-GRANTED-FORM 3.pdf

855-KOLNP-2007-GRANTED-FORM 5.pdf

855-KOLNP-2007-GRANTED-SPECIFICATION-COMPLETE.pdf

855-KOLNP-2007-INTERNATIONAL SEARCH REPORT & OTHERS.pdf

855-kolnp-2007-others.pdf

855-KOLNP-2007-PETITION UNDER RULE 137.pdf

855-KOLNP-2007-REPLY TO EXAMINATION REPORT.pdf


Patent Number 256467
Indian Patent Application Number 855/KOLNP/2007
PG Journal Number 25/2013
Publication Date 21-Jun-2013
Grant Date 19-Jun-2013
Date of Filing 09-Mar-2007
Name of Patentee FIRMENICH SA
Applicant Address 1 ROUTE DES JEUNES, P.O. BOX 239, 1211 GENEVA 8
Inventors:
# Inventor's Name Inventor's Address
1 TROPHARDY, GIL 607, RUE DU PRE DE L'ETANG, 01170, GEX,
2 VERHOVNIK, GLENN 225, ROUTE DE PRE DE MALAGNOU, 1224, CHENE- BOUGERIES,
PCT International Classification Number A61K8/11
PCT International Application Number PCT/IB2005/053089
PCT International Filing date 2005-09-20
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 04104835.6 2004-10-01 EUROPEAN UNION