FR3109733A1 - PERFUME IN THE FORM OF A DRY POWDER AND USE OF POWDERS FOR THE PREPARATION OF A COMPLEX PERFUME - Google Patents

Abstract

The invention relates to the field of perfumes in solid and dry form. More particularly, the invention relates to a process for preparing a perfume in powder form from a liquid, semi-liquid or pasty odorous matrix. The scent matrix can be of an artificial or natural nature. The process combines steps of extraction, gas dissolution, cryogenics and lyophilization. The perfume powder can be used in free or compact form.

Description

PERFUME IN DRY POWDER FORM AND USE OF POWDERS FOR THE PREPARATION OF A COMPLEX PERFUME

The invention relates to the field of perfumes in solid form. More particularly, the invention relates to a process for preparing a perfume in the form of a dry powder from a liquid, semi-liquid or pasty fragrant matrix. The odor matrix can be artificial or natural in nature. The process combines extraction, gas dissolution, cryogenics and freeze-drying steps. The perfume powder can be used in free or compact form.

Field of invention

Solid perfumes as we know them today are generally composed of an odorous material available in liquid, semi-liquid or pasty form mixed with a waxy and/or fatty type solid support.

Unlike liquid perfumes, solid perfumes can be formulated without alcohol, which eliminates the strong smell characteristic of alcohol-based perfumes and offers softer and more persistent perfumes. The absence of alcohol also avoids the risk of the appearance of spots following exposure to the sun.

Solid perfumes made from concrete flowers appeared at the beginning of the 20th century, but essential oils are also widely used to prepare solid perfumes. The odorous matrix must be sufficiently concentrated to be perceived once mixed with the solid support, the concentration having to be low enough so that the solid state of the support is preserved.

However, the solid perfumes currently available have drawbacks due to their formulation from fatty or waxy products. Their manipulation is likely to stain the materials with which they come into contact, in particular clothing. They lubricate the skin and due to a melting point slightly above room temperature, they do not remain solid in heat, for example when exposed to the sun.

Solid perfumes, although subject to growing interest in the world of perfumery, remain marginal due to these drawbacks.

There is a real need to have new formats of solid perfumes and new processes for preparing such perfumes.

The inventors have developed a process for preparing a solid perfume in dry form from an odorous matrix in the form of a dehydrated powder.

This process consists, from a liquid, semi-liquid or pasty odorous matrix, in:

1. Dissolving a gas in the said matrix by passing through a zone dense in gas molecules, such a density being obtained (i) either thanks to a gas flow generated by the evaporation of a cryogenic fluid, (ii) or by an elevation pressure;
2. Cryogenize said gas-rich matrix obtained in step a) under pressure and temperature conditions making it possible to maintain said trapped gas to obtain frozen granules, particles or beads;
3. Lyophilize said granules, particles or beads to obtain a dehydrated powder.

The invention also relates to the perfume powder obtained by such a process, in the form of loose powder or compressed powder, compacted or formed in any other way.

The invention relates to both solid perfumes obtained from a single matrix and complex solid perfumes obtained by mixing several powders, as well as their method of preparation and a perfume compact in which are placed one or more perfumes under free or compact form.

Advantages of the invention

The present invention makes it possible to prepare high quality perfumes in a novel format.

The perfumes according to the invention are solid and dry; they come in the form of a dehydrated powder that can be compressed to order. Thus, they can be offered in the form of a loose powder or a compact powder. The compact powder can take different forms: block to be placed in a compact, but also balls or pebbles. This modularity makes it very easy to use.

Perfumes in solid form are very interesting for perfumers who have a new fragrant material with high quality while being stable over time. These perfumes offer new perspectives in the design of perfumes.

They can be produced without any support (which is technically possible if the matrix is appropriate) but a neutral support is advantageously added at the time of the freeze-drying to fix the odors and for questions of processability. The support plays a dual role by providing dry matter: (i) fixing the odorous volatile compounds and (i) fixing the oily fraction of the plant extracts. Thus, the volatile compounds are captured in their diversity and the smell of the powder is faithful to that of the original matrix. In addition, the oily fraction of plant extracts whose melting temperature is only slightly above room temperature, remains in a dry form regardless of the temperature. The perfuming product in dry solid form is stable at temperature both from a formulation and olfactory point of view.

This support is advantageously chosen from molecules commonly used for this purpose such as maltodextrins or from natural supports such as rice powder or other natural powder. Prepared in this way, the powders meet the most restrictive standards of cosmetics, as well as the expectations of consumers who are looking for products that are not dangerous to their health.

The starting odorous matrix can be of any type, which gives access to a very wide olfactory field. Solid perfumes can be obtained from perfumes formulated in liquid form then transformed into powder, for example to extend a range of perfumes into derivative products. Notably, the inventors have shown that the solid perfume retains all the notes (head, heart and base) of the initial perfume.

It should be noted that the extraction process makes it possible to produce a fragrant powder from any type of plant material and, remarkably, from dumb flowers, these flowers from which no technique has so far made it possible to extract the odors. yet highly sought after in perfumery such as lily, violet, peony, lily of the valley, wisteria and so many others. Thanks to the invention, the artisan perfumer has a wide range of natural fragrant extracts to create new perfumes.

The inventors have in fact observed that the smell contained in these solid ingredients faithfully reproduces the smell of fresh plant matter and that this smell lasts for a very long time without altering. The odorous ingredients therefore have significantly improved properties compared to the solid odorant extracts available until now.

These perfume powders also make fragrant raw materials for the creation of personalized perfumes accessible to any uninitiated user.

The solid perfumes made available by the present invention therefore have many advantages both in terms of their ease of use, transport and preservation as well as their olfactory quality and the creativity to which they give access. Their presentation in the form of a compact gives access to a new way of wearing perfume.

Finally, the method for preparing such solid perfumes is simple, rapid, industrializable and inexpensive.

DETAILED DESCRIPTION OF THE INVENTION

A first object of the invention relates to a method for preparing a perfume in solid and dry form from a liquid, semi-liquid or pasty odorous matrix comprising the steps of:

1. Dissolving a gas in the said matrix by passing through a zone dense in gas molecules, such a density being obtained (i) either thanks to a gas flow generated by the evaporation of a cryogenic fluid, (ii) or by an elevation pressure;
2. Cryogenize said gas-rich matrix obtained in step a) under pressure and temperature conditions making it possible to maintain said trapped gas to obtain frozen granules, particles or beads;
3. Lyophilize said granules, particles or beads to obtain a dehydrated powder.

The dissolved gas can be an inert gas such as nitrogen, argon... or a non-inert gas such as CO2 or nitrous oxide, or a mixture of gases. When it is desired to protect the matrix against oxidation, a particularly preferred cryogenic fluid is liquid nitrogen.

By the terms “under pressure” within the meaning of the invention, we mean conditions which allow the dissolution and/or the trapping of a gas in a matrix and/or its maintenance in the said matrix during freezing. The pressurization can be obtained either by raising the pressure, or by bringing the matrix into contact with a cryogenic fluid, the evaporation of this gas creating a density of gas molecules equivalent to a pressurization so gas molecules dissolve in the matrix.

When the dense zone of molecules is obtained by an increase in pressure, this pressure is greater than atmospheric pressure, and may in particular be greater than 0.5 bar, 1 bar, 2 bars, 5 bars, 10 bars, 50 bars, 100 bars, 200, bars, even 250 bars or more. In a particular embodiment, it is between 2 and 100 bars. For the sake of clarity, it is specified that the pressures expressed in this document correspond to relative pressures, i.e. atmospheric pressure is considered as a pressure of 0 bar.

In a preferred embodiment, the zone dense in gas molecules is obtained at least in part thanks to a flow of the gas generated by the evaporation of a cryogenic fluid. It can be obtained by combining the evaporation of a cryogenic fluid with an increase in pressure. The terms "a flow of gas generated by the evaporation of a cryogenic fluid" cover the flow resulting directly from the evaporation of a cryogenic fluid as well as any controlled flow (direction, flow rate, etc.), by injection of gas or by suction for example, which allows the creation of one or more exchange zones between the matrix and a large number of gas molecules.

The pressure and temperature conditions applied in step b) must make it possible to maintain the gas trapped in the matrix in step a). Those skilled in the art will know how to adjust the pressure and temperature conditions during step b), so that the solubility of the gas in the matrix is greater than or equal to that implemented during step a). Said solubility is in particular influenced by the temperature (for gases it increases when the temperature decreases) and by the pressure (equilibrium of the partial pressures between the matrix and the gas).

Thus, steps a) and b) take place under correlated conditions (between these two steps) in order to allow the dissolution of the gas in the matrix and its conservation inside the matrix during cryonics.

Preferably, the steps of the method are carried out one after the other and in particular the freeze-drying step is implemented immediately after the cryogenic step. Moreover, the process is preferably carried out continuously. However, it is possible to keep the intermediate product obtained at the end of the cryogenic stage in frozen form and to carry out the freeze-drying later, after a negative cold storage time to keep the products in the solid state (for example at -20°C).

The process conditions can be adapted according to the shape of the matrix to be dehydrated, in particular the pressure during the cryogenic stage, and the freeze-drying parameters. A person skilled in the art will know how to make such adaptations.

Advantageously, when the odorous matrix is of plant origin, it is quickly transferred to the gas dissolution and cryogenics apparatus in order to limit the degradation or denaturation of the compounds.

By "fragrant matrix" is meant any matrix that can be used to produce a perfume without limitation of origin or state, except that it must be supplied in a liquid, semi-liquid or pasty form in order to be able to be treated by the process according to the invention. This matrix may contain alcohol as in the case of a perfume formulated in liquid form (for example a commercial perfume) which it is desired to transform into a solid perfume. It can also be of natural origin and in particular be made up of 100% plant material.

Thus, in a particular embodiment of the invention, the odorous matrix is a liquid perfume containing alcohol.

In another embodiment of the invention, the odorous matrix is exclusively composed of plant material. It can consist of a single plant material or a mixture of several plant materials.

The plant materials that can be used are chosen for example from flowers or parts of flowers such as petals, pistils, leaves, stems, but also from herbaceous plants such as aromatic herbs, fruits of any type such as raspberries, lychees, apples, vanilla pods or roots such as ginger, or spices. The plant material is preferably fresh, or freshly cut, so that the odorous molecules are not altered, and the smell emanating from the plant material is as close as possible to the natural state.

In a particular embodiment, the plant material is from a dumb flower such as lily, violet, hyacinth, duddleia, peony, freesia, lily of the valley, honeysuckle, gardenia, carnation, pittosporum, mock orange, sweet pea, wisteria and heliotrope.

Thus, a second object of the invention relates to a perfume powder in free form. This powder may contain a support which ensures the handling of the powder (fineness, volatile nature) but also to fix the odorous molecules for long-term quality. A vegetable powder such as rice powder can be used for this purpose, but other carriers such as maltodextrins are also suitable and commonly used. The holder allows the powder to be calibrated to ensure consistent quality (standardization).

The method according to the invention can also comprise a step of compressing the dehydrated powder obtained by freeze-drying to provide a compact powder.

The perfume format in the form of a compact powder facilitates the handling of the powder and its dosage by artisan perfumers, but also its use by the consumer.

A third object of the invention relates to a method for preparing a complex solid perfume by mixing at least two powders in free form as defined above.

By "complex perfume" within the meaning of the invention, is meant a solid perfume obtained by mixing at least two perfume powders obtained by the preparation process as defined above.

It should be noted that each of these powders can correspond to a single odor (from a single plant or a single fruit for example) or be from a mixed matrix (mixture of several plant materials or synthetic perfume) . Thus, a perfume powder before mixing can itself take on a certain olfactory complexity.

The mixture of these odors can be achieved by the artisan perfumer or by the consumer who wishes to create a unique perfume. No technical constraint linked to the invention limits the type of mixture that can be produced.

Thus, a fourth object of the invention relates to a solid perfume in compact form obtained by compression of a perfume powder in free form as defined above or of a mixture of loose powders obtained by the method defined above.

Although solid perfume can be in the form of a loose powder (format used in perfumery and cosmetics), it is generally easier to handle a compact powder.

A powder in compact form or "compact powder" or "compressed powder" or formed in any other way differs from a powder in free form or "loose powder" by the fact that it can be handled without the powder volatilizing . The degree of compaction does not matter and will be adapted to the use. For example, a compact powder intended to be placed in a perfume compact must be compact enough to remain attached to the box when the latter is turned over and the compression must at the same time allow the perfume powder to be removed by simple effleurage with the powder brush or cosmetic sponge. Those skilled in the art will be able to adapt the compression parameters to this use.

A fifth object of the invention relates to a perfume compact comprising at least one solid perfume.

The solid perfume is obtained by the process according to the invention of preparing a solid perfume then placing the dry compact powder in the compact. The solid perfume can be placed directly in free or compact form after compression of the dehydrated powder. In a preferred embodiment, it is in compact form.

The compact can include one or more compartments containing a perfume.

In a first particular embodiment, the compact comprises a customizable perfume consisting of a main perfume and at least one auxiliary perfume making it possible to modulate the smell of the main perfume. This auxiliary perfume can correspond to one of the notes of the main perfume or to an additional note.

In a second particular embodiment, the compact comprises the different notes making up a defined perfume, separated, making it possible to recompose said perfume while operating variations of balance according to the desire of the user.

In a third particular embodiment, the compact is suitable for creating a personalized perfume. It includes different perfume powders allowing different perfume mixing tests to be carried out to achieve a tailor-made result, which can then be reproduced in the form of a personalized complex perfume by mixing the selected powders. Preferably, the number of powders offered in such a compact will be greater than 3, more preferably greater than 5, and even more preferably greater than 10 and may be increased without any particular limit up to 20, 30, 40, 50 or even more, depending on the diversity of the palette that you want to make available.

According to these three embodiments, the invention relates to a perfumery compact comprising several separate locations in which are arranged either (i) a main perfume and at least one auxiliary perfume, or (ii) different perfumes corresponding to the different notes composing a perfume complex, or (iii) different perfume powders.

The solid perfumes which are the subject of the invention can be used as body perfumes, but also as room perfumes in free form for "powdering" furnishing fabrics or for dispersing in the air.

A sixth object of the invention relates to the use of a perfume powder as defined above for perfuming a cosmetic composition.

Such a cosmetic composition may for example be a foundation powder such as a foundation in the form of a loose or compact powder.

The present invention is illustrated with the aid of the examples which follow, these should in no way be considered as limiting the scope of the present invention.

Figure 1: Chromatograms obtained following analysis by a Heracles II electron nose from AlphaMos (double ultrafast gas chromatography) of the lilac powders prepared by applying the extraction process according to the invention (A: column 1; B: column 2) .

EXAMPLES

EXAMPLE 1: Preparation of lilac powders

Preparation process

White lilac and purple lilac flowers were harvested and processed separately.

The petals were separated from the flowers manually before being passed through an ANGEL 7500 horizontal juice extractor. The juice thus harvested was immediately treated in equipment allowing it to be cryogenized while trapping dissolved gas in it, according to the process described in patent WO2019/234341 for example. The frozen beads thus obtained were then freeze-dried under conventional conditions in a CHRIST alpha 1-8 freeze-dryer, until “dry” powders were obtained (no more weight loss measured).

Characteristics of powders

The first remarkable element comes from the quantity of powder thus obtained. For the two treated flowers, the powder yields were around 5%, which is very high since no support was added and it is therefore only material initially present in the petals. Freeze-drying supports are generally added to the preparations to be freeze-dried, in order to guarantee the presence of a sufficient dry extract for the fixation of molecules of interest during processing and also to reduce production costs. The yield obtained during this preparation is already very convincing on these two points without the need to add anything.

The second very remarkable element is the smell of the products thus obtained, which were very clearly identified as being those of the two respective flowers by the various panels consulted. Electronic nose analyzes (Figures 1A and 1B) also made it possible to confirm the presence in the product of characteristic peaks associated with chemical compounds known to be significant contributors to the scents of lilac flowers:

• (E)-ocimere, which is the major component;
• lilac aldehydes and lilac alcohols, which have several dimers each and are among the most characteristic compounds;
• benzyl methyl ether, 1,4-dimethoxybenzene and indole, which are the other characteristic compounds of lilac fragrance.

Peaks were identified on the chromatograms using their retention indices on each column. The reference data used are those of the software coupled with the Heracles II measuring device and the NIST WebBook available in particular from the address: https://webbook.nist.gov/chemistry/#Search.

Since the lilac is one of the so-called "dumb" flowers, it is all the more remarkable to have succeeded in obtaining, in relatively large quantities, a product which conforms in terms of smell and which can be used as ingredients for perfumery or cosmetic.

EXAMPLE 2: Preparation of jasmine powders

Jasmine flowers were collected. The petals and pistils were separated manually before being passed through an ANGEL 7500 horizontal juice extractor. method described in patent WO2019/234341 for example. The frozen beads thus obtained were then freeze-dried under conventional conditions in a CHRIST alpha 1-8 freeze-dryer, until “dry” powders were obtained (no more weight loss measured). In the other juice fractions, representing 200g each, 50g of maltodextrins were added each time, then the mixtures thus obtained underwent the same process as described above, until powders were obtained.

The powder yields thus obtained are:

• about 5% for the petals without added maltodextrins;
• approximately 10% for the pistils without added maltodextrins;
• around 30% for the petals with the addition of maltodextrins;
• about 35% for the pistils with added maltodextrins;

All the products obtained offer a smell very similar to that of the starting flower.

The choice of whether or not to add a support such as maltodextrins depends on the starting matrix and the quality of product sought. For some products, the dry powder alone can become liquid again, this is particularly the case when the oily fraction is too high; it is then necessary to add a support at the time of freeze-drying. On the other hand, by adding a support, the yield is increased as illustrated above, which is advantageous economically, and allows the standardization of the products.

EXAMPLE 3: Preparation of a solid perfume from a commercial perfume composition

Preparation process

100g of a classic perfume concentrate (liquid and containing alcohol) was emulsified in 900g of demineralised water according to the process described in patent WO2010/149668, so as to obtain an emulsion containing no surfactant. The preparation thus obtained was then textured using an addition of 6g of xanthan gum and then 100g of maltodextrins were added to the preparation, in order to serve as a support for freeze-drying. The product was then treated in equipment making it possible to cryogenize it while trapping dissolved gas therein, according to the method described in patent WO2008/043909, under a pressure of 4 bars. The frozen beads thus obtained were then freeze-dried under conventional conditions in a CHRIST alpha 1-8 freeze-dryer, until “dry” powders were obtained (no more weight loss measured).

Characteristics of powders

The powder thus obtained clearly has the same perfume as the original product and the derivative products which are derived from it, such as the finished and marketed perfume.

Furthermore, reimplementation tests were carried out by applying the powder obtained by the present process to the previously wet skin of volunteers. On another skin area, the commercial perfume in liquid form was applied. After application, the two perfumed areas of skin have very similar odors, which is already remarkable given that the powder prepared using the method described in the present application no longer contains ethanol (removed during the step of lyophilization), which is known and used to serve as a vector and support for perfuming compounds.

After a few minutes to tens of minutes, the commercial perfume begins to fade, while the powder perfume persists without weakening. This difference is more and more pronounced as time goes by. This phenomenon is also particularly remarkable and unexpected, as alternative solutions to the use of ethanol are generally inefficient in terms of odor retention over time.

Claims (10)

Process for preparing a perfume in solid form from a liquid, semi-liquid or pasty fragrant matrix comprising the steps of:

1. Dissolving a gas in said matrix by passing through a zone dense in gas molecules, such a density being obtained (i) either thanks to a gas flow generated by the evaporation of a cryogenic fluid, (ii) or by an elevation pressure;
2. Cryogenize said gas-rich matrix obtained in step a) under pressure and temperature conditions making it possible to maintain said gas trapped in order to obtain frozen granules, particles or beads;
3. Freeze-drying said granules, particles or beads in order to obtain a dehydrated powder.

A method according to claim 1 wherein said odor matrix is a liquid perfume containing alcohol. Process according to Claim 1, in which the said odorous matrix is exclusively composed of vegetable matter. Process according to one of Claims 1 to 3, in which the said dehydrated powder is compressed. Perfume powder in free form obtained by the process as defined in one of claims 1 to 3. Process for the preparation of a complex solid perfume by mixing at least two powders as defined in claim 5. Solid perfume in compact form obtained by compression of a perfume powder as defined in claim 5 or of a mixture of powders obtained by the process defined in claim 6. Compact perfumery comprising at least one solid perfume as defined in one of claims 5 or 7. Compact according to claim 8 comprising several separate locations in which are arranged either (i) a main perfume and at least one auxiliary perfume, or (ii) different perfumes corresponding to the different notes making up a complex perfume, or (iii) different perfume powders . Use of perfume powder as defined in claim 5 for perfuming a cosmetic composition.