DE102010046931A1 - Process for the preparation of a cosmetic product - Google Patents

Abstract

The invention relates to a method for filling a preparation which is solid at room temperature and which is formed from a first phase and a second phase and contains at least one thermolabile ingredient, comprising the process steps of heating the second phase, dissolving the thermolabile ingredient in the first phase, and heating the first phase to a temperature which substantially corresponds to the temperature of the second phase, the first phase being heated in the conveying path to a mixer which then mixes the first phase with the second phase to form the preparation.

Description

The invention relates to a process for the liquid hot filling of a solid at room temperature preparation, which is formed from a first phase and a second phase. Furthermore, the invention relates to a product prepared by the process, which can be filled in any shape and in any donor forms.

In the preparation of preparations, such as emulsions, in particular of oil-in-water emulsions, various processes are involved, from the preparation of the oil and water phase, the mixing of the two phases by means of an emulsifier to an emulsion, to the filling of the emulsion in small containers, such as pens , Jars or tubes known. Such methods can be subdivided into at least two groups. The first group relates to processes for making and filling solids such as creams and lotions which over a wide temperature range, i.a. a. even at room temperature, can be filled into appropriate donor forms. The second group relates to processes in which the product to be prepared is solid at room temperature, so that a liquid filling is possible only in a heated state. The present invention is directed to the second group of high temperature liquid filling processes.

Furthermore, the methods differ with regard to the respective constituents of the preparations, since these react differently to individual process steps. In hot filling in particular thermolabile substances play a major role, which decay into parts over a too long period of time when too high a temperature. In the case of the decomposition of thermolabile ingredients, unwanted by-products may also possibly arise. The method according to the invention is applicable in all fields of technology, in particular if a preparation of two phases is to be produced, which has a thermolabile ingredient. The invention is further defined by means of a foot care agent in solid form (stearate gel), which has urea (urea) as a thermolabile ingredient.

Basically, it is known that due to age- or disease-related increasing dryness of the skin of the feet excessively cornea forms, which can lead to painful tears (so-called rhagades). Conventional cosmetic preparations for relieving this skin problem are exclusively creams. In order to meet the skin care claim, such creams are very greasy (eg water-in-oil emulsion). This has the distinct disadvantage that after applying the hands are also very greasy, which is perceived by a variety of users as extremely unpleasant. However, cleaning the greasy hands by hand washing is only possible with difficulty due to the place of application on the foot. The freshly applied cream would either be incorporated into the carpet when running or even lead to slippery floors even a considerable risk of injury from slipping.

From the prior art, a variety of manufacturing processes are known. For example, the DE 10 2008 028 821 A1 a method for producing a cosmetic stick, wherein the wax and oil components are heated together with the oil-in-water emulsifier to 90 ° to 95 ° and melted, then the also heated from 90 ° to 95 ° water with the water-soluble active - And ingredients is added with vigorous stirring, if necessary, further ingredients are added, the mixture is cooled to a suitable filling temperature, filled into suitable dispensing forms and solidified by static cooling (without further stirring) to room temperature.

The DE 196 43 238 A1 discloses a manufacturing method of cosmetic sticks, wherein in a so-called. One-step process, the water phase is added to the hot fat phase and then cooled to room temperature.

From the DE 24 22 903 a manufacturing method is known in which fat and water phase are kneaded at 65 °. However, this is not enough to obtain a homogeneous stick composition based on an oil-in-water dispersion.

It is disadvantageous in the prior art processes that both phases are strongly heated from the beginning and hot-worked throughout the entire production process. In this case, thermolabile substances would disintegrate after a certain time above their critical temperature into parts and possibly form unwanted by-products. Consequently, such processes can only be used if the thermolabile substances were not supplied from the beginning, but only during the cooling phase below a critical decomposition temperature. This is possible, for example, with certain creams and lotions and with a small proportion of the thermolabile substance, but not with products which have a high proportion of thermolabile substances and / or which are already solid at room temperature. Furthermore, it is not possible to add the thermolabile ingredients to such products during the cooling phase, since adequate mixing in a rapidly solidified preparation is not ensured and the thermolabile ingredient would not be homogeneously dispersed in the preparation.

In the production of creams, sticks, etc., in principle, large quantities are pre-produced, which are then bottled in a filling system in small donor forms with recording sizes of for example 25 g. In order to operate the production process economically, preparation quantities of at least 1500 l are prepared, the filling of which takes many hours to days. In any case, the filling time is significantly longer than the time until a thermolabile material would disintegrate at the temperatures of the prior art manufacturing processes. It is impossible to add the thermolabile of the 80 ° to 90 ° hot emulsion to be prepared without the material hydrolyzing to bottling. Consequently, only the first products of the respective batch of bottling would contain undecomposed thermolabile substances. The following units could also be burdened with decomposition by-products and thus become unusable. A further problem is that solidification and renewed remelting strongly influence the galenic properties and the structure formation of the solid to be produced (eg a stearate gel stick), so that the preparation preprocessed to a sufficiently great extent is melted, stored and only gradually can be bottled.

In the example of a foot care product containing urea as a thermolabile ingredient, not only a break-up occurs in parts at the temperatures of the prior art, it also develops the pungent-smelling ammonia as a by-product.

Based on this, it is the object of the invention to provide a method, with which large quantities of a room-solidifying preparation can be produced, which contains a thermolabile ingredient, it being ensured that the entire batch of packaged packings has the ingredient and this during the Production process does not decompose.

This object is achieved by a method for filling a at room temperature (20 ° C) solid preparation, which is formed from a first phase and a second phase and contains at least one thermolabile ingredient, the first phase at room temperature liquid and the second phase at Room temperature is fixed. The method comprises the following method steps. Heating the second phase to a temperature T ₂ high enough so that the second phase is liquid, dissolving the thermolabile ingredient in the first phase at a temperature T ₁ that is below the critical temperature value of the at least one thermolabile ingredient and below the temperature T ₂ is located. Heating the first, the thermolabile ingredient-containing phase to a temperature T ₁₂ , which substantially corresponds to the temperature T _{2 of} the second phase, wherein the heating of the first phase in the conveying path to a mixer, which then the first phase with the second phase for Formulation of the preparation at a temperature which essentially corresponds to T ₁₂ .

By means of the method according to the invention, both the first and the second phase can be prepared independently of one another in large quantities in collecting containers, the first phase with the thermolabile ingredient being provided clearly below the critical temperature value. A "critical temperature value" is to be understood as meaning the temperature at which the thermolabile ingredient begins to disintegrate or the disintegration can be detected by means known from the prior art. For example, the decomposition of urea can be tested by means of an odor test, since the ammonia produced during the decomposition can be detected already at an odor threshold value of 3.5 mg per cubic meter of air. It is particularly favorable to heat the first phase containing the thermolabile ingredient in the conveying path in the region of the mixer, the "conveying path" being defined as the section between the mixer and the storage container of the first phase. Conveniently, a heating device may be provided directly on the conveyor tube, so that the first phase is heated during the flow through the conveyor tube, but it may also be provided to flow the first phase in a separate heater in which they are heated and then into the flow tube is returned. Due to the spatially close connection of the heater for heating the first phase of the mixer, the time required for filling can be kept as short as possible. The process according to the invention can provide an aqueous solution as the first phase and a fatty phase as the second phase. Alternatively, as a second phase, a preparation can be used in which fat contents are mixed with water by means of emulsifiers. A mixture of the first phase containing the thermolabile ingredient is then made into an emulsion to produce a thermolabile ingredient formulation. The phases are mixed and bottled in the liquid state. In the present case, this generally applies as "liquid", which is flowable, ie, for example, has a viscosity of less than 10,000 mPa · s at 20 ° C, for stearate gels preferably about 100 mPa · s at 80 ° C.

In the method according to the invention is favorable that the filling of the preparation at a filling temperature T ₃ is carried out, which is so high that the preparation is liquid and at the same time is reduced so that the cooling of the preparation takes place in the filled state as quickly as possible. By the liquid filling on the one hand any donor forms can be filled without air inclusions, on the other hand, the cooling in the bottled state, preferably in small quantities, without additional cooling influences from the outside fast enough to the to preserve thermolabile material. To accelerate the cooling and even safer preservation of the thermolabile ingredient is favorable to provide at least one cooling tunnel in the filling line. If at least one cooling tunnel is used, in a likewise favorable embodiment the temperature T3 downstream of the mixer may even be greater than or equal to the temperatures T ₂ or T ₁₂ .

According to the invention, the method is such that the time between the heating of the first thermolabile ingredient-containing phase over the critical temperature value of the at least one thermolabile ingredient and the cooling of the preparation below the critical temperature value is less than the thermolabile ingredient begins to disintegrate. The two phases can be prepared independently of time and temperature and provided in any quantity. By heating the first phase just before the mixer, the time to cool down can be kept very low. It ensures a processing time from the heating of the first phase to the cooling of the total preparation below the critical temperature value of less than 15 minutes. In the case of urea as a thermolabile ingredient thus disintegration and the associated ammonia formation can be avoided.

In a favorable embodiment, a static mixer or oscillation mixer can be used as mixer, with which a homogeneous merging of the first and second phase is ensured. At the same time, a heating device can be provided on the mixer, which heats the first and second phases during the mixing process and effects an equalization of the temperatures.

Further preferred is an embodiment in which the heating of the first phase containing the thermolabile ingredient to a temperature T ₁₂ takes place immediately before the mixer. As "immediately before" is a spatial proximity to the mixer of less than three meters of the conveying path to the mixer, a temporal proximity of less than 30 seconds, until the first and second phases flow into the mixer. The heating can be ensured by a heating device integrated in the conveying path, which is arranged so close to the mixer, that said temporal and spatial sizes can be achieved. In this way, the thermolabile material is exposed to the high temperatures above the critical temperature for a particularly short time.

For the smooth filling of several thousand small containers (donor forms) per hour, it can be conveniently provided that the mixed preparation is taken before filling in a storage container having 50-500 times the volume of the small container. Usually, the small container sizes of 20 to 150, in exceptions, between 5 and 500 ml.

In a favorable embodiment of the invention, the second phase is heated to a temperature of T ₂ of at least 80 ° C, the first, the thermolabile ingredient-containing phase to a temperature T ₁₂ of 75 to 85 ° C. After heating the first phase, the streams of both phases are combined and fed into the mixer. Alternatively, the phases can also be separated up to the mixer and brought together in the mixer. After mixing, the preparation passes into the storage container in which the temperature can already be lowered to a filling temperature T ₃ , which thus maintains the temperature T _{12 of} the first heated phase. By reducing the temperature, the tendency to disintegrate or decay of the thermolabile ingredient is reduced to a minimum.

In the following, the method according to the invention will be explained in more detail, without being limited thereto, by means of an exemplary embodiment shown in the figures.

1 shows a schematic representation of the method according to the invention the example of a pedicure in solid form (stearate), which has urea as a thermolabile ingredient.

A first phase 1 and a second phase 2 are each provided in large quantities of over 700 liters, with the first phase 1 an aqueous solution of water, urea and allantoin. The second phase consists essentially of water, magnesium aluminum silicate, propylene glycol, panthenol, NaOH solution and stearic acid. Since the stearic acid and the silicate are in a solid state at room temperature, the second phase is heated to a temperature T ₂ so that it becomes liquid. The temperature T ₂ reaches at least 80 ° C, preferably 80-85 ° C. In the aqueous solution of the first phase 1 the thermolabile ingredient urea is already dissolved. The temperature T ₁ must therefore be significantly lower than the temperature T _{2 of} the second phase 2 to prevent disintegration of the thermolabile ingredient. To avoid the crystallization of the urea, the temperature T _{1 is} at least 40 ° C.

The first phase 1 is by means of a pump 8th' , the second phase 2 by means of a pump 8th in the direction of a mixer 4 pumped. In the illustration shown, the first and second phases 1 . 2 before entering the mixer 4 merged. With a dashed line, the alternative solution is shown, in which the first phase 1 and the second phase 2 immediately in the mixer 4 merged and mixed there. Before the Merging the first and second phases 1 . 2 For example, the temperatures of the phases are substantially equalized, with the first phase containing the thermolabile ingredient urea 1 by means of a heating device spanning the conveying path 7 is heated to a temperature T ₁₂ , which is substantially the temperature T _{2 of} the second phase 2 equivalent. In the embodiment shown, the temperature T _{2 of} the second phase 2 vary in a range of 80 to 90 ° C, the temperature T _{12 of} the first phase is therefore at about 80 ° C. The mixture of the first and second phase 1 . 2 to form the preparation, ie the final product 3 occurs at a temperature substantially equal to T ₁₂ . To quickly cool the preparation 3 To prevent this, which would lead to an excessive increase in viscosity and filling problems would entail, the mixer 4 also be provided with a heater.

After mixing in the mixer 4 will the preparation 3 a storage container 5 fed, which has a storage capacity of about 10 kg, to a continuous filling in small containers 6 at a filling rate of 2,000 pieces per hour. Without the use of a storage container 5 Ensuring a uniform filling quantity would be considerably more difficult. In the reservoir 5 the preparation has a filling temperature T ₃ , which is below the temperature T _{12 of} the first phase 1 as well as the preparation 3 in the mixer 4 lies. Preferably, the filling temperature T _{3 is} approximately equal to 70 ° C.

The inventive method is designed such that the period between the heating of the first, the thermolabile ingredient urea contained phase 1 by means of the heater 7 about the critical temperature of the urine and the cooling of the preparation 3 below the critical temperature value is smaller than that of the thermolabile ingredient urea decomposes. For urea, this time is in particular a maximum of 15 minutes. The filling of the preparation 3 , which has a melting point of 60 ° C (rising melting point ASU L 13.00-21), in small containers 6 takes place in the liquid state, the cooling of the preparation then follows within the small container in the filled state.

Heating the first, the thermolabile ingredients Urea contained phase 1 from a temperature T ₁ to a temperature T ₁₂ by means of the heating device 7 takes place immediately before the mixer 4 , wherein immediately in the illustrated embodiment means that the heater 7 essentially at the mixer 4 subsequently arranged and the first phase 1 in a few seconds from the heater 7 in the second phase 2 and to the mixer 4 flows. The heater 7 is in the example shown within three meters of the conveyor to the mixer 4 arranged so that the first and second phases flow into the mixer within 30 seconds after heating the first phase. To realize these values, the respective pipe diameter of the conveying path in the embodiment shown is 3 cm, the volume flow through the pumps 8th . 8th' is a total of 60 l / h.

Although not explicitly illustrated, it is understood that the pumps 8th . 8th' , the heater 7 , the static mixer 4 , as well as the filling device are connected to a control or regulation, by means of which the flow velocities, the temperatures and all the rest are controlled to ensure a continuously uniform process flow necessary influencing variables.

The invention is not limited in its execution to the above-mentioned preferred embodiments. Rather, a number of variants is conceivable, which makes use of the illustrated solution even with fundamentally different types of use. For example, the reservoir 5 be provided with a heater to keep the filling temperature constant.

QUOTES INCLUDE IN THE DESCRIPTION

This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.

Cited patent literature

• DE 102008028821 A1 [0005]
• DE 19643238 A1 [0006]
• DE 2422903 [0007]

Claims (13)

Method for filling a preparation solid at room temperature ( 3 ) from a first phase ( 1 ) and a second phase ( 2 ) and contains at least one thermolabile ingredient, comprising the steps of: - heating the second phase ( 2 ) to a temperature T ₂ which is so high that the second phase ( 2 ) is liquid, - dissolving the thermolabile ingredient in the first phase ( 1 ) at a temperature T ₁ which is below the critical temperature value of the at least one thermolabile ingredient and below the temperature T ₂ , - heating the first, the thermolabile ingredient-containing phase ( 1 ) to a temperature T ₁₂ substantially equal to the temperature T _{2 of} the second phase ( 2 ), wherein the heating of the first phase in the conveying path to a mixer ( 4 ), followed by the first phase ( 1 ) with the second phase ( 2 ) for the preparation of the preparation ( 3 ) at a temperature substantially equal to T ₁₂ . A method according to claim 1, characterized in that the filling of the preparation takes place at a filling temperature T ₃ , which is so high that the preparation ( 3 ) is liquid and the cooling of the preparation takes place in a bottled state. Method according to at least one of the preceding claims, characterized in that the time interval between heating up the first, the thermolabile ingredient-containing phase ( 1 ) over the critical temperature value of the at least one thermolabile ingredient and cooling the preparation ( 3 ) below the critical temperature value is smaller than that of the thermolabile ingredient decays, in particular maximum 15 minutes. Method according to at least one of the preceding claims, characterized in that the mixture by a static mixer ( 4 ) or an oscillation mixer. Method according to at least one of the preceding claims, characterized in that the heating of the first, the thermolabile ingredient-containing phase ( 1 ) to a temperature T ₁₂ immediately before the mixer ( 4 ) he follows. Method according to at least one of the preceding claims, characterized in that the mixed preparation before filling into a Vorratsbehalter ( 5 ) and the filling into small containers ( 6 ), which have a volume of 5 to 500 ml. Method according to the preceding claim, characterized in that the storage container ( 5 ) 20 to 500 times the volume of small containers ( 6 ) having. Method according to at least one of the preceding claims, characterized in that the heating of the second phase ( 2 ) to a temperature T ₂ of at least 80 ° C. Method according to at least one of the preceding claims, characterized in that the heating of the first, the thermolabile ingredient-containing phase ( 1 ) to a temperature T ₁₂ of 75 to 85 ° C. Method according to at least one of the preceding claims, characterized in that a filling temperature T _{3 of} the preparation ( 3 ) below the temperature T _{12 of} the heated first phase ( 1 ) lies. Method according to at least one of the preceding claims, characterized in that the dissolution of the thermolabile ingredient in the first phase ( 1 ) at a temperature T ₁ of at least 40 ° C and a maximum of 45 ° C. Method according to at least one of the preceding claims, characterized in that the thermolabile ingredient is urea and / or allantoin. Product prepared according to at least one of the preceding claims.

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