DE19548067A1 - Deodorant product and process for its manufacture - Google Patents

Abstract

A solid shaped alum-based deodorant product containing fragrances or essential oils is produced by exposing to a sufficiently strong microwave radiation a mixture of 50-99 % by weight of a double salt of formula (I) M<I>M<III>(SO4)2.12H2O, in which M<I> stands for an alkali or ammonium ion and M<III> stands for an aluminium, titanium, manganese, iron or chromium ion; 0.1-30 % by weight of auxiliary agents to improve the esthetic, cosmetic or processing properties, including 0.1-20 % by weight of a fragrance or essential oil, and optionally up to 40 % by weight of other water-soluble aluminium salts in a microwave-permeable form. Exposure to microwave radiation is continued until the mixture is heated and at least partially melted or sintered. It is then left to cool down and solidify.

Description

The invention relates to a deodorant product based on alum, which contains Contains fragrances or essential oils and with the help of microwave technology in the form of a largely transparent to clear molded body is obtained.

Alum is a collective name for a group of double salts, of which the potassium alum KAl (SO₄) ₂ · 12 H₂O is best known and because of its astringent and antiseptic Properties has found application in medicine and pharmacy. It is also knows that alum has deodorant properties. Has antiperspirants and deodorants one uses alums in powder form or in the form of the so-called alum stones. alum has the properties of melting in crystal water (potassium alum at around 92 ° C, ammonium mood at approx. 95 ° C, sodium alum at approx. 60 ° C). The melts are pourable and can be shape as you like in this way.

From EP-A-157 736 a method is also known, a potassium stone from an alum block by cutting out a cylindrical pin. Formulations for production hemostatic pens based on alum are various cosmetic manuals remove, e.g. B. from "The Chemistry and Manufacture of Cosmetics" (Maison G. de Navarre, 2nd edition 1975) pages 707-708 or "Cosmetics, Science and Technology" (Edward Saga rin, 2nd edition, 1972), and 2, pages 34-35 or "Textbook of Cosmetics" (Edmund Schrümpf, 3rd ed., 1974), page 336.  

From the French patent FR 2 575 922 a pasty deodorant Composition based on a 50% solution of alum in water and with a Ge known of 5 wt .-% perfume.

However, none of the previously known methods allows the production of fragrances the tempering pencils, since the melting of the alum in their own crystal water according to conventional Chen process must be done very carefully and slowly so that the water of crystallization does not take off distilled and evaporate the volatile fragrances to a large extent during this process would. Sensitive fragrance components would be affected by the high temperature discolor or decompose load. In any case, unsightly, cloudy and little smell obtained deodorant moldings.

However, a certain fragrance content is very advantageous for use as a deodorant and it there was therefore a great interest in obtaining alum pencils containing fragrances which have an attractive appearance and not only when used on the skin develop an antiperspirant effect, but at the same time existing smells cover slightly. It has now been found that these problems can be solved by to make such a deodorant using microwave technology.

The invention therefore relates to a solid, shaped and preferably transparent deodo rant product with a content of 50 to 99 wt .-% of a double salt of formula I.

M ^I M ^III (SO₄) ₂ · 12H₂O

in which M ^{I is} an alkali or ammonium ion and M ^{III is} an aluminum, titanium, manganese, iron or chromium ion and, if appropriate, salt up to 40% by weight of further water-soluble aluminum and with a fragrance or ethereal Oil in an amount of 0.5 to 20 wt .-%, based on the entire product, and optionally up to 10 wt .-% further auxiliaries.

Instead of the uniform double salts, mixtures of different double salts can also be used be included under the general formula I group. Mixtures of simple salts from which the double salts are composed can be used. So can e.g. B. also a mixture of 1 mole of K₂OSO₄ and 1 mole of Al₂ (SO₄) ₃ · 18 H₂O and 6 moles of H₂O or from 0.5 mol Na₂SO₄, 0.5 mol K₂SO₄, 1 mol Al₂ (SO₄) ₃ · 18 H₂O and 6 mol H₂O be det. The double salts of formula I are formed from these mixtures when heated under the influence of microwave radiation.

The deodorant product according to the invention preferably contains at least 80% by weight of a double salt of the formula I in which M ^{I is} sodium, potassium or NH₄⁺ and M ^{III is} aluminum. Other water-soluble aluminum salts, which may be present in the deodorant products according to the invention in an amount of up to 40% by weight, are preferably the products already known as astringents, such as aluminum sulfate (Al₂ (SO₄) ₃ · 18H₂O), aluminum chloride (AlCl₃ · 6 H₂O), aluminum hydroxychloride (Al₂ (OH) ₅Cl · 2-3H₂O), aluminum chlorate (AlClO₃) ₃ · 9 H₂O), aluminum formate, aluminum acetate, aluminum potassium sulfophenylate, aluminum naphtholsulfonate and aluminum sodium acetate. These further aluminum salts are preferably only present in small amounts up to 20% by weight in the deodorant products according to the invention.

By adding one or more of these aluminum salts to the invention Deodorant products can have the astringent and antiseptic properties of Products are still increasing.

As fragrances, individual fragrance compounds, such as. B. Linalool, Geraniol, Aceto phenol, lilial, geranonitrile, dihydromyrcenol, o-tert-butylcyclohexyl acetate, phenylethyl alcohol hol, benzophenone, rose oxide, methyl benzoate, α-hexyl cinnamaldehyde, vetiveryl acetate, 8- Dodecactone, allylamylglycolate, hydroxycitronellal, benzyl acetate or amylbutyrate be set. However, mixtures of different odoriferous substances are preferably used create an appealing fragrance together. Such perfumes can also be natural  Fragrance mixtures, such as those obtainable from plant or animal sources, contain The amount of fragrance contained depends on the intensity of the desired Fragrance and according to the volatility and fragrance intensity of the perfume. A lot of 1 to 10 As a rule,% by weight should be sufficient.

Also essential oils, which are usually less volatile, but often have an additional antimi have a crobial or skin-care effect, instead of or preferably in addition to the actual fragrances can be contained in the deodorant products according to the invention. Suitable essential oils are e.g. B. chamomile oil, sage oil, clove oil, rose oil, lemon balm oil, min zen oil, linden blossom oil or juniper berry oil.

Other auxiliaries in an amount up to 10 wt .-% in the deodo according to the invention rant product can be included, serve the further aesthetic and cosmetic Aus equipment as well as its processing and durability.

So it can be a clear and easy incorporation of the fragrances or the essential oils be advantageous to dilute them with suitable auxiliaries and make them dispersible or adsorb them on powdery carriers with a high surface area and place them on them Way to make it more distributable. Suitable tools for this purpose are e.g. B. one or polyhydric alcohols with 2 to 6 carbon atoms, e.g. B. isopropanol, propylene glycol, glycerin, Sorbitol, polyethylene glycol or surfactants e.g. B. oxyethylated sorbitan fatty acid esters, oxyethylated Fatty acid partial glycerides, ethylated castor oil, fatty alcohol polyglycol ether, alkyl (oligo) glycosides or mixtures of such products.

Suitable powdered carriers are e.g. B. pyrogenic silica (Aerosil®), talc, Bentoni te or other finely divided silicates. Other tools that improve the appearance of the Deodorant products according to the invention are dyes and pigments. So z. B. water-soluble dyes or pigments, preferably pearlescent, with TiO₂ be layered mica pigments can be added.  

To improve the cosmetic effect, skin care or anti-inflammatory Active ingredients such as As urea, allantoin, panthenol, antioxidants such. B. ascorbic acid, Hydroxycarboxylic acids such as. B. lactic acid, glycolic acid or citric acid or other Kos Metically effective substances such as B. phytic acid, amino acids or tretinoin can be added.

Water-soluble polymers such as As polyvinyl pyrrolidone, polyvinyl alcohol or polyethylene glycol cole can be added to further improve the deodorant effect. Close Lich can also lanolin, oil components such. B. almond oil and silicone oils in small menus gene added.

Finally, it has proven beneficial to have a small amount of free, not in the alum grid to have bound water in the educt. This water makes the dielectric loss factor tor - this is a measure of the energy that the material is exposed to under microwave radiation takes - increases and the time it takes to produce a homogeneous melt, further lowered. In general, an amount of 0.5 to 5% by weight of water is sufficient. The This proportion of free water also serves to prevent small losses of water of crystallization can occur during the melting process by evaporation, replaced and which can crystallize alluvial meadows with the full hydrated water shell.

The process described for the preparation of the deodorant products according to the invention The base of alum salts is not only used to incorporate volatile components such as e.g. B. of fragrances but generally represents an advantageous way to help tel to improve the aesthetic, cosmetic and processing properties ten such as B. essential oils, dyes, pigments, skin care, dermatologically effective or cosmetically interesting substances, oil components or processing technology helpful Incorporate components homogeneously and gently into these products. This is mainly because the fact that the microwave radiation heats the mixture "from the inside", as it the Molecules for rotation according to their dipole moment, in particular water molecules and thus stimulates the transfer of energy to the neighboring molecules.  

In contrast, heat transfer by heating from the outside is considerably slower and leads to a significantly higher thermal load on all components, which is reflected in the Evaporation of volatile components and in the decomposition of unstable active substances shows and increases a reduction in the color and smell of the end product.

Another subject of the invention is a process for the preparation of the solid, shaped deodorant product, in which a mixture of
50-99% by weight of a double salt of the formula I.

M ^I M ^III (SO₄) ₂ · 12H₂O (I)

in the M ^I an alkali or ammonium ion and
M ^{III is} an aluminum, titanium, manganese, iron or chromium ion,
0.1-30% by weight of auxiliaries for improving the aesthetic, cosmetic or processing properties and, if appropriate
exposes up to 40% by weight of further water-soluble aluminum salts in a form permeable to microwaves to radiation with microwaves with sufficient energy until the mixture heats up and at least partially melts or sinters, and then, after the microwave radiation has ended, cools down.

In this method, the cosmetic aids, e.g. B. fragrances gentle and ho mogen incorporated and received a product of good transparency. It is preferred here Add a small amount of approx. 0.5-5% by weight of water to the mixture, so that the small Amounts of water that evaporate from the melting or sintering process be compared.

The radiation with microwaves takes place in a vessel which is permeable to microwaves, e.g. B. in glass, ceramics or plastics. The process of Irradiation, melting and cooling in the packaging of the deodorant product, e.g. B. in a pin sleeve. Any plastic that is up to a temperature that is about 10-20 ° C above the melting temperature of the deodorant Product, shows no softening or decomposition. The inner surface of the vessel  ßes or the form in which the microwave radiation takes place, should be smooth so that the Allows the product to be easily removed from the mold after cooling.

The mixture of the double set, the auxiliaries and possibly the other water-soluble ones Aluminum salts should be relative even before melting under microwave radiation be homogeneous and finely divided. This can be done e.g. B. achieve this by having the fixed com components, primarily the salts, in finely ground form, solid auxiliaries in powder form, liquid in the form of low viscosity and easily dispersible solutions or emulsions or adsorbed to powdery carrier inserts and to a homogeneous premix with each other mixes. The more homogeneous the mixture of components before the microwave Irradiation, the more homogeneous and transparent the deodo according to the invention is obtained rant product after the melt has cooled. As microwaves are within the scope of the Erfin to understand electromagnetic wave rays whose frequency is in the range between 3 and is 300,000 MHz. This range covers the frequency range of the radio waves from 3 to 300 MHz and that of the actual microwaves from 300 to 300,000 MHz.

Irradiation is preferably carried out with microwaves at a frequency of 2450 MHz. The recipe-specific high-frequency output is a maximum of 1500 watts / kgh before draws less than 500 watts / kgh.

The duration of irradiation with microwaves, which creates a homogeneous melt the components required depends on the set power of the microwave System and on the amount, the homogeneity of the premix and the melting point and the dielectric loss value of the premix, and, if the microwel len system is a belt system, depending on the belt speed.

However, it has been shown that when using a microwave device with 2450 MHz at a Power of 250 watts to generate a melt from a sample of approx. 50 g of potassium mood (with a content of approx. 2% by weight of free water) only a radiation duration of 2-4  Minutes is required to produce a homogeneous crystal melt. The following case Games are intended to explain the subject of the invention in more detail.  

Examples Preparation of the premix

A liquid mixture was made from perfume oil, propylene glycol, dyes and water (Examples 1-3 and 5).

For example 4, a powdery premix was prepared from perfume oil, water and Aerosil posed.

Production of the deodorant product

The fine crystalline alum (KAl (SO₄) ₂ · 12 H₂O, particle size 0.01-0.5 mm) was with the liquid premix (in the case of Example 4 with the powder premix) under Stir mixed until a homogeneous distribution of the components was achieved (about 3 minutes ten).

The alum mixture obtained was placed in a pencil case with a capacity of 50 g filled, the lid screwed on and the filled pen sleeve with the cap towards un into an MLS 1200 microwave oven from MLS with a microwave oven 2450 MHz. There the samples were run for 2 minutes Irradiated 250 watts. After the samples had cooled, they were turned over and the lid unscrewed. It was found that solid, clear or transparent, e.g. T. colored (Examples 2, 3 and 5) Products with a smooth surface in the shape of the inside of the ver end cap were obtained.

The recipes can be found in the following table (all figures in% by weight):

The following perfume oil compositions were used:

• A: AFF 7683 (fragrance mixture from Azur Fragrances)
• B: 94-754 (fragrance mixture from HENKEL KGaA)
• C: AF 947649 (fragrance mixture from Azur Fragrances)

The following dyes were used:

• (a) 0.3% Blue No. 1, 0.1% solution
• (b) Williams Red 10 B, No. 33, 0.1% solution.

Claims (5)

1. Solid shaped deodorant product with a content of 50-99 wt .-% of a double salt of the formula (I) M ^I M ^III (SO₄) ₂ · 12H₂O (I) n the M ^I an alkali metal or ammonium ion and M ^{III is} aluminum, titanium, manganese, iron or chromium ion and optionally up to 40% by weight of further water-soluble aluminum salts, characterized in that a fragrance or an essential oil in an amount of 0.1 to 20 % By weight and optionally up to 10% by weight of further auxiliaries are contained. 2. Deodorant product according to claim 1, characterized in that it contains at least 80 wt .-% of a double salt of formula I in which M ^{I is} sodium, potassium or NH₄⁺ and M ^III aluminum. 3. Deodorant product according to claim 1 or 2, characterized in that 1 to 10 % By weight of a fragrance are contained. 4. A process for the production of solid, shaped, transparent deodorant products, characterized in that a mixture of
50-99 wt .-% of a double salt of the formula M ^I M ^III (SO₄) ₂ · 12 H₂O in which M ^{I is} an alkali or ammonium ion and M ^{III is} aluminum, titanium, manganese, iron or chromium ion is
0.1-30% by weight of auxiliaries for improving the aesthetic, cosmetic or processing properties and, if appropriate
exposes up to 40% by weight of further water-soluble aluminum salts in a form which is permeable to microwaves and is irradiated by microwaves with sufficient energy until the mixture warms up and at least partially melts or sinters and then, after the end of the microwave irradiation, allows it to cool and solidify . 5. The method according to claim 4, characterized in that the irradiation with a recipe-specific high-frequency output of maxinial 1500 watts / kgh, preferably less than 1000 watts / kgh and most preferably less than 500 watts / kgh carries out.