CH713127B1 - Synthetic scented material and its manufacturing process. - Google Patents

Abstract

The present invention relates to a scented synthetic material characterized in that it comprises a zeolite powder impregnated with an essence giving the synthetic material its fragrance.

Description

Object of the invention

The present invention relates to a new synthetic material diffusing a fragrance over a long time scale. It also relates to the process for manufacturing said synthetic material.

Technological background

[0002] Many consumers appreciate scented objects whether for deodorant purposes or to bring a certain atmosphere to a room. Often these are spongy bodies such as paper or felt impregnated with perfume.

[0003] In general, these scented objects have the drawback of losing their scent power in a few weeks. To remedy this drawback, several compositions have been developed in the field of synthetic materials. For example, document FR 2 743 566 discloses a polymer resin of the polyether-esteramide type containing a perfumed composition with at least two volatile aromatic components.

[0004] Despite innovations in this field, the interest in the development of scented synthetic materials diffusing their fragrance over a time scale extending over several months, or even over several years, is still very present. The development of these new products and the related processes requires not drastically modifying the process parameters and not modifying the final properties of the product as well as its aesthetic appearance (surface homogeneity, smooth structure without cracks, color retention. wanted, etc.).

Summary of the invention

The object of the present invention is to develop a synthetic material diffusing a perfume over a long time scale, namely several months, or even several years.

[0006] It also aims to develop a method for manufacturing this new synthetic material that does not alter the final properties of the material, whether in terms of resistance or of aesthetic appearance.

[0007] For these purposes, a material, a product and a method according to the appended claims are provided.

Brief description of the figures

The invention will be illustrated below in more detail with the aid of the appended drawing, given by way of non-limiting example.

[0009] FIG. 1 respectively represents the chromatogram of a perfumed sample according to the invention before and after the accelerated aging test. The baseline represents the chromatogram of the unscented reference polymer.

Detailed description of the invention

The present invention relates to a scented synthetic material and its manufacturing process. By synthetic material is meant plastics and elastomers. Natural rubber is included in synthetic materials. The synthetic material incorporates in its formulation a zeolite powder comprising in its pores an essence giving the final product a fragrance which desorbs over a time scale of at least one year.

The manufacturing process consists in mixing the raw synthetic material, a natural or synthetic essence prepared by matching on the basis of a fruit, an eau de toilette, a material (leather, wood, etc.) , etc. Before mixing, the essences are deposited beforehand on zeolite. They can, for example, be deposited on the zeolite by spraying in the liquid phase at room temperature so that the perfume molecules are adsorbed in the pores of the zeolite. The scented zeolite powder is then incorporated into the green synthetic material. The incorporation can, for example, be carried out in a roller mixer without heating the rollers. Still by way of example, the mixing speed can be between 2 and 10 m / min with a roller spacing of between 0.5 and 3 mm and a mixing time of between 5 and 15 minutes. Besides the synthetic material, the formulation can include the vulcanization system, certain additives and colored pigments. Conventionally, the polymerization can be carried out in a press or by injection.

Zeolite refers to a porous aluminosilicate crystal which can, according to the invention, be of several types (mordenite, etc.). For example, it can be a clinoptilolite which is a porous arrangement of silica and tetrahedral aluminum with a monoclinic crystal system.

The zeolite has a pore size of between 1 and 200 Å, preferably between 1 and 100 Å, and more preferably between 1 and 10 Å measured by physical adsorption (physisorption). It has a BET specific surface area of between 10 and 1000 m <2> / g, preferably between 30 and 800 m <2> / g and more preferably between 200 and 700 m <2> / g. It has an average particle size (d50%) of between 0.5 and 30 μm and, preferably, between 1 and 10 μm.

Gasoline can be formed from different chemical compounds such as esters, aldehydes, ketones to name a few. It is advantageously oil-based and can reproduce any type of odor (fruity, musky, etc.). The gasoline content relative to the zeolite powder is between 1 and 70%, preferably between 10 and 50% and more preferably between 20 and 40% by weight. In the final material, the gasoline content is between 0.5 and 20%, preferably between 1 and 10% and more preferably between 2 and 5% by weight.

The perfumed zeolite powder has a content relative to the synthetic material of between 2 and 40%, preferably between 2 and 30%, more preferably between 3 and 15% and even more preferably between 3 and 8% by weight.

The synthetic material is chosen as a function of the application, that is to say of the targeted product. It may, for example, be a rubber, a silicone or a thermoplastic and, more particularly, in the latter case, a thermoplastic from the family of polyolefins (polyethylene, etc.), d 'a polyamide, polypropylene, POM (polyoxymethylene) or else a polyurethane-based thermoplastic. Advantageously, the synthetic material is a rubber, and preferably an FKM rubber (class of fluoroelastomers). In the case of a watch strap, an FKM rubber is preferably chosen because it offers the advantage of having a silky feel, excellent ultimate mechanical properties, of being protected against UV and ozone, and adaptable for a facilitated implementation. However, the present invention does not exclude the use as a synthetic material of an HBNR rubber, i.e. an elastomer based on nitrile-butadiene or else other elastomers such as an NBR or EPDM elastomer, and the like.

As mentioned above, watch straps can in particular be made with this new scented material, but any type of product is possible. We can cite, by way of example, boxes (soap boxes, etc.), jewelry, ornamental pieces, floor or table coverings, and, in general, accessories of all kinds such as a scented key ring, a scented rubber insert for a handbag, a stopper for a flask or bottle, a shoe sole, etc. Mention may also be made of products intended for food, such as straws or cups.

The advantages of the scented material according to the invention are now illustrated through the non-limiting examples described below.

Examples

Experimental procedure

The tests focused on scented FKM rubbers and on a non-scented reference. Two clinoptilotite zeolite powders from Lithos Industrial Minerais with different particle sizes were tested. A first powder (Lithofill MM) has an average particle size (d50%) of 2 µm and a second powder (Lithofill BM) has an average particle size (d50%) of 6 µm. Both powders have, according to their technical data sheets, a pore size of 4 and a specific surface area of between 400-600 m <2> / g. The perfumed samples comprise the same essence which is a mixture of esters giving off an odor of fruit and, in particular, of damask. Specifically, gasoline includes ethyl esters of decanoic acid, ethyl esters of dodecanoic acid and ethyl esters of hexadecanoic acid.

Table 1 below shows the samples tested. Perfume content (wt%) 0 2.5 2.5 5 5 Zeolite content (wt%) 0 5 5 6.6 6.6 d50 zeolite powder (µm) / 2 6 2 6

Table 1

The reference sample (REF) is FKM rubber with the vulcanization system, without perfume. Samples 1 and 2 were prepared with a zeolite powder / gasoline mixture comprising respectively 66% by weight of zeolite powder and 33% gasoline. In the two samples, the content of the zeolite powder / gasoline mixture is 7.5% by weight. The differences between samples 1 and 2 are that they are produced with zeolite powder having an average particle size d50 (%) of 2 and 6 μm respectively. Samples 3 and 4 have a higher gasoline content with a zeolite powder / gasoline mixture comprising respectively 57% by weight of zeolite powder and 43% gasoline, with a mixture content in the samples of 11.6% by weight . As previously, samples 3 and 4 are differentiated by the mean size d50 of the particles of the zeolite powder with a size of 2 and 6 μm respectively. The samples were prepared as follows. The scent essence and the zeolite powder were mixed at room temperature. This mixture was incorporated into the rubber using a roller mixer. The baking was then carried out in a press at 170 ° C. for 12 min. A post-treatment at 175 ° C for 2 hours was carried out to remove residues.

The shore A hardness of the samples was measured according to the ASTM D412C standard. Aging tests were carried out for sample 2 subjected to exposure to ultraviolet light (SUNTEST) according to standard SN EN ISO 105-B02: 1994 + A2: 2000. The tests were carried out for 30 hours and simulate exposure to light for one year. After accelerated aging, a headspace analysis with solid phase preconcentration was performed. This method allows the analysis of volatile and semi-volatile substances and is suitable for evaluating the intensity of a perfume. In this method, we measure the amount of substances released by the sample, that is to say contained in the headspace when the sample is positioned in a vial. Specifically, a 9cm <2> polymer fragment is sealed in a 20ml headspace vial for analysis. The vial is sealed with a silicone septum cap and heated for 20 minutes at 60 ° C. The VOCs released are then extracted on a solid phase (INDEx, Tenax) and analyzed by gas chromatography with detection by mass spectrometry (GC-MS). The molecules detected are identified by comparison with a spectra library (NIST). The concentrations of the scent molecules are evaluated by the intensity of the 88 ion which is characteristic of ethyl esters. The intensity is compared between a sample which has not undergone aging and a sample which has undergone the 30 hour aging treatment.

Results

From an aesthetic point of view, no change in the appearance of the samples was observed: no cracks or any visible inhomogeneity on the surface. In terms of properties, Table 2 gives the Shore A hardness of the samples. Shore A 72 70 72 71 71

Table 2

Little difference is observed between the reference sample and the samples comprising perfumed zeolite powder, the values remaining of the order of 70.

The headspace analysis focused on sample 2 which has the lowest percentage of gasoline (2.5% compared to 5% for samples 3 and 4). FIG. 1 represents respectively the chromatogram of this sample before and after the aging test. The analysis shows that UV irradiation results in a loss of volatile VOCs but no change in the composition of the gasoline. Peaks 5, 6 and 7 respectively relating to ethyl esters of octanoic acid, decanoic acid and dodecanoic acid are present before and after aging. After aging, the reduction in concentration of all the ethyl esters is 79%. From a sensory point of view and in the case that interests us from an olfactory point of view, the intensity scales are logarithmic. This means that a decrease in the concentration of scent molecules by 80%, results in the nose by only a decrease in the intensity of the scent by 10%. It will also be specified that the headspace analysis only measures the substances given off by the sample and not those contained inside the sample, which are not easily accessible under the conditions of the test. Therefore, even if the odor has diminished after the test, new odorous molecules may subsequently diffuse from the inside to the outside of the sample, causing stabilization, or even a slight increase in the odor. In summary, these tests demonstrate that after one year, the scented synthetic material retains a significant odoriferous power despite a fragrance content in the material limited to 2.5% by weight.

Claims (10)

1. Fragrant synthetic material, characterized in that said material is a silicone, a thermoplastic or a rubber comprising a zeolite powder impregnated with an essence giving the synthetic material its fragrance. 2. Material according to claim 1, characterized in that the gasoline content in said material is between 0.5 and 20%, preferably between 1 and 10% and more preferably between 2 and 5% by weight. 3. Material according to claim 1 or 2, characterized in that the zeolite powder has a pore size between 1 x 10 <-10> and 2 x 10 <-8> m, preferably between 1 x 10 <-10 > and 1 x 10 <-8> m and more preferably between 1 x 10 <-10> and 1 x 10 <-9> m. 4. Material according to any one of the preceding claims, characterized in that the zeolite powder has an average particle size d50 of between 0.5 and 30 microns and preferably between 1 and 10 microns. 5. Material according to any one of the preceding claims, characterized in that the zeolite powder has a specific surface area of between 10 and 1000 m <2> / g, preferably between 30 and 800 m <2> / g, and more preferably between 200 and 700 m <2> / g. 6. Material according to any one of the preceding claims, characterized in that, in said material, the content of zeolite powder impregnated with gasoline is between 2 and 40%, preferably between 2 and 30%, more preferably. between 3 and 15% and even more preferably between 3 and 8% by weight. 7. Material according to any one of the preceding claims, characterized in that said rubber is a fluoroelastomer. 8. Product comprising the material according to any one of claims 1 to 7. 9. Product according to claim 8, characterized in that said product is a watch strap. 10. A method of manufacturing a scented synthetic material according to one of claims 1 to 7 comprising the steps of: - Adsorption of a zeolite powder with an essence; - Mixing of the adsorbed zeolite powder with a formulation comprising a plastic material or a respectively raw elastomer; - Polymerization of the mixture to produce said scented synthetic material.