RU2419414C1 - Method of obtaining emulsion cosmetic preparation - Google Patents

Abstract

FIELD: medicine.

SUBSTANCE: invention relates to field of cosmetology and represents method of obtaining emulsion cosmetic preparation, including step-by-step dispersion in solvent at room temperature of poorly soluble components, components being introduced into installation with powerful hydroacoustic impact, in which carried out are dispersion of components and cavitation homogenation of emulsion with further packing, characterised by the fact that mode of resonance acoustic cavitation is formed inside flowing mechanic fluctuation system-canal of rectangular section with larger side a and smaller side b respectively, generation of acoustic fluctuations is realised in phase on both opposite sides a with amplitude exceeding threshold of acoustic cavitation for moving multi-phase medium, consisting of mixed ingredients, amplitude of fluctuations is selected optimal for different stages of emulsion preparation, frequency f of acoustic fluctuations is selected equal to resonance frequency of entire canal with elements of added mass, which is determined by any known method, smaller distance b between canal walls is selected multiple to one fourth of wavelength, excited in said multi-phase medium, where f is frequency of generated fluctuations, Hz, C is sound velocity in multi-phase medium, m/s, b is distance between canal walls, m.

EFFECT: invention ensures obtaining the finest monodisperse cream emulsions with submicronic size of disperse phase, coalescence-resistant.

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Description

The invention relates to the field of cosmetology and dermatology and can be used in biology, pharmacology, the cosmetic industry, veterinary medicine and the food industry, in particular in cosmetology - in the development of technologies for producing cosmetic products for skin, nail and hair care.

It is known that penetration into the deeper layers of the skin of biologically active substances, including, depends on the size and homogeneity of the oil phase of the cosmetic cream, which includes vegetable and essential oils, a number of important extracts and other fat-soluble ingredients. As a rule, in the technology of obtaining cream, they tend to break the oil phase into droplets of the smallest possible size.

In this case, together with the liposomes of the oil-in-water emulsion, biologically active components can penetrate through the layers of the epidermis dissolved in the oil phase of the emulsion, sorbed on the interface.

A known method of obtaining cosmetic cream, comprising the following stages of the process:

- weighing and melting of raw materials;

- preparation of the fat and water phase;

- emulsification;

- cooling and perfume;

- packaging in packaging containers.

To prepare the aqueous phase, the ingredients are heated to 75-80 ° C. To prepare the fat phase, the ingredients are heated to 80-85 ° C. Next, the fat and water phases are mixed. Under certain conditions (temperature, pH, order of entry), DNA and preservatives are added to the cream mass (RF patent No. 2032399, IPC A61K 7/00, A61K 7/48). The disadvantage of this method is the significant energy consumption of the technology for producing the cream and the decrease in the biological activity of its components during the preparation of the product due to the fact that the process of obtaining the emulsion occurs when heated to 80-85 ° C, then there is a homogenization of two phases, which makes it difficult to introduce components and additives critical thermal decomposition (temperature no more than 40-45 ° С) and at the same time necessary for homogenization. These disadvantages significantly limit the scope of this method, in particular for the preparation of emulsions (creams, lotions, etc.) containing natural vitamin supplements.

A known method of obtaining a cosmetic product in the form of an emulsion, which includes preparing the base by dispersing vegetable oil, emulsifier and glycerin in a dispersion medium, followed by introducing biologically active substances of plant and animal origin into the emulsion during mixing. A polyethylene oxide gel is used as an emulsifier, and dispersion is carried out at room temperature (RF patent No. 2126247, IPC 7 A61K 9/10, 7/48, publ. 2001). The disadvantage of this analogue method is that, to intensify the processes of dissolution and dispersion, as well as to obtain thin emulsions and suspensions, containers are additionally equipped with high-speed mixers. Another disadvantage of this method is the impossibility of carrying out a homogenization process (cold emulsification) while biologically active substances are introduced into the cream in order to obtain an emulsion with submicron particle size.

The closest in technical essence to the present invention is a method for producing a cosmetic product in the form of an emulsion, comprising dispersing in a solvent at room temperature poorly soluble components, an emulsifier and biologically active substances (of any origin), solid powdery ingredients (sorbents or abrasives), the components being administered simultaneously or sequentially through individual dispensers directly into the sounding chamber of the rotor-cavitation installation, where The process of cavitation emulsification is studied while passing through the sound chamber of the Mirra emulsion complex (or any other) and an aqueous solution (RF Patent No. 2240782, IPC 7 A61K 9/10, A61K 9/50, A61K 9/127, A61K 7/48 , 2004).

The essence of the invention is to use the principle of cavitation homogenization (emulsification) to obtain highly effective environmentally friendly cosmetic and therapeutic cosmetic emulsion products. There is no doubt that the use of the method of rotary-cavitation treatment to obtain emulsion cosmetics has several advantages over traditional methods of emulsification.

However, the process, or rather the mode, of rotor-cavitation homogenization in the sounding chamber of rotary devices requires additional detail.

It is known [1] that different modes of cavitation of sound waves can be implemented in practice in the sounding chamber and in the channels of the stator of a rotary installation. Formulations such as “rotary-cavitation installation with powerful sonar action” and “mixture .... which are produced in the rotary-cavitation installation by the method of cavitation emulsification” need to be specified. The question is only about the optimal choice of operating modes of rotary-cavitation units, since they depend on many factors. For example [/ 1 /, clause 2.2.2] technically, the device implements the cavitation mode for almost all pressure differential values, however, this can result in both hydrodynamic cavitation mode [/ 1 /, clause 2.1.4] and acoustic cavitation mode. Moreover, the features of resonance phenomena in rotary devices include the presence of many resonances [/ 1 /, clause 1.1] and their complex relationship with the design parameters of the installation, operating modes, and media characteristics. Each structural element is a generator of its frequency spectrum, which ultimately overlap (superposition) on each other. In section 4.4, the author [1] proved that the process of dissolving sulfur in a mixture of oils is optimal under the operating mode of a rotary apparatus, when it is acoustic pulsed cavitation that is excited in it.

A number of design solutions of the rotor-stator pair and input pipes for tuning to resonant frequency superposition for a certain technological process are proposed. One of the authors of the prototype method in an interview [5] says that the frequency of exposure during rotor-cavitation homogenization is three times higher than the frequency of the current in the electric network, i.e. has the order of 150-180 Hz. According to the results of [/ 1 /, clause 2.2.4], this is probably one of the resonance modes, and there are resonances at higher frequencies with a higher spectral density and better quality factor, in particular, resonance frequencies of ~ 540-580 Hz are noted.

Thus, we can note the following significant disadvantages of the prototype:

- a difficult choice of the optimal operating mode of the rotary-cavitation installation to obtain the required dispersion and homogeneity of the final emulsion;

- the limitation on the highest possible resonant frequency, which in practice does not exceed ~ 2000 Hz, due to the complex structure with many parts, each of which is an emitter of oscillations, which ultimately overlap each other and not always in phase;

- in practice, it is known / 6 / that after passing through a homogenizer in an emulsion, the process of coalescence (fusion) of the droplets of the dispersed phase occurs, even if the initial droplet size is small and amounts to tens of nanometers, the result is a stable emulsion, but with a wide distribution spectrum of the size of the dispersed phase in size.

Figure 1 presents a photograph after processing with a digital filter "smart sharpness" cream manufactured by ZAO Mirra-M (Nourishing Cream with Medicinal Herbs), obtained using an optical microscope with a magnification of 1000 times and a digital nozzle with a resolution of 5.2 megapixels. To assess the size of the dispersed phase, an object micrometer was used (Figure 2) with a division price of 10 μm. To process digital images, the Image Scope application was used. The differential size distribution of the dispersed phase (processing results) is shown in FIG. 3. As can be seen from the obtained results, the rotor-cavitation homogenizers used by Mirra cannot ensure the long-term stable existence of a dispersed phase of ~ 500-600 nm in size, which is considered close to optimal for human skin, although the fraction of this phase may be higher immediately after the homogenization process.

Investigations of more than 40 different creams (direct and reverse emulsions) of leading Russian and foreign manufacturers conducted by DERMANIKA showed that the size distribution of the dispersed phase of all companies is close to each other (the difference is no more than two times the size of the main mode) and determined by the types of rotor homogenizers used.

In addition, the studies performed allowed us to determine the optimal energy and frequency characteristics of acoustic vibrations in the treated emulsion to obtain significantly better indicators for the size of the dispersed phase and the stability of the emulsion, to obtain correlation between the size of the dispersed phase and frequency, as well as the level of homogeneity and the quality factor of the oscillatory system - channel. Effective methods have been found to bring the peroxide number (characterizes the amount of free radicals) to regulatory requirements. Part of the research was reported at the XIV International Scientific and Practical Conference "Cosmetics and Raw Materials: Safety and Efficiency" in October 2009, where they are awarded second place and diploma, there are publications in specialized journals / 7 /.

The resonance regimes of a near-plane (quasi-plane) standing acoustic wave in a flowing emulsion in a rectangular channel are realized (the channel length is much greater than the distance between the side walls). In this case, in accordance with the criteria (threshold) of cavitation [2-4] and operation in the resonant mode with maximum efficiency, the best indicators are provided for the intensification of combined physicochemical, hydromechanical, heat and mass transfer processes on the medium to be processed and the minimum size obtained at the output and homogeneity of the fat (oil) phase.

This technology was implemented on an industrial scale at the existing cosmetic enterprise "CJSC EMANSI Laboratory". A photograph of an industrial installation is shown in FIG. 4. The first products manufactured using this technology - Anti Smell Smoke hand cream (for smokers, against the effects of nicotine and smoke on the skin of the hands), passed the whole cycle of certification tests (sanitary and epidemiological conclusion No. 77.01.12.915.P.006156.02.10 of 03.02 .2010 and the Declaration of Conformity, which are duplicated by independent tests in the Spectrum laboratory (accreditation certificate No. РОСС RU.0001.21ПШ50) with the corresponding protocol No. 19 dated 12/22/2009.

The aim of the invention is to reduce the average size of the dispersed phase upon receipt of any type of emulsion (direct and inverse), improve homogeneity (uniformity in size).

This goal is achieved by the fact that the regime of a quasi-plane resonant wave and acoustic cavitation is formed inside a flowing mechanical oscillating system-channel of rectangular cross section with a large side a and small side b, respectively, sound waves are generated in phase on both opposite sides a with an amplitude exceeding the acoustic cavitation threshold for a moving multiphase medium consisting of mixed ingredients, and the vibration amplitude is selected optimal for various s emulsion preparation, and the frequency f of sound vibrations is selected to equal the resonant frequency of all channel elements associated mass as determined by any known method, the minimal distance b between the walls of the channel selected multiple of a quarter wavelength, is excited in the multiphase medium:

b = (k / 4) * (C / f), k = 1,2,3, ...,

where f is the frequency of the generated oscillations, Hz;

C is the speed of sound in a multiphase medium, m / s;

b is the distance between the walls of the channel, m

As an example, we give the characteristics and tuning order of the flow channels used in the industrial installation of Figure 4.

The determination of the natural frequencies of complex profile structures with an attached mass is a non-trivial task, especially since we are talking about vibrations of the ultrasonic frequency in the range of ~ 25-50 kHz. In this regard, after a theoretical calculation, carried out, for example, according to the technique of / 8 /, as a rule, several refinement steps are required to fine-tune the resonant frequencies and obtain the required quality factor.

The authors use their own methodology, which is based on a large accumulated material on instrumental measurement of the vibration spectrum of rectangular channels. Figure 5 presents a typical vibration spectrum of the channel in the form of a cartridge, which is used in an industrial installation. For measurements, the measuring path, verified in ROSTEST, consisting of a piezo-accelerometer type 4344 and an amplifier 2635 from Bruel & Kjaer, a digital oscilloscope Velleman with a fast Fourier transform function with registration of signals to a personal computer, is used. A linear scale with an upper resolution of 60 kHz is used. It is clearly seen that this design has a main resonant frequency of ~ 24.5 kHz (marked with a marker). The second noticeable resonance at a frequency of ~ 54 kHz coincides with the passport data of the 4344 type piezo-accelerometer - this is its own resonant frequency. To excite oscillations, it is at this frequency that a specially developed ultrasonic frequency generator with automatic frequency control is used. The next stage of tuning is the choice of piezoelectric emitter frequencies and the geometry of their attachment to the channel-cassette. Accordingly, the frequency of the piezo emitters is selected as close as possible to the resonant frequency. In this case, it was 24.6 kHz with an input power of 100 W per emitter, which ensured a stable cavitation mode during the flow of a multiphase medium - the basis of cosmetic emulsion at the first stage of preparation. As a multiphase medium, a typical formulation of one of the creams of the company COGNIS (Optimal Face Cream) consisting of:

PHASE 1 Emulgade se 4.0% Cutina cbs 1,0% Lanette o 1,0% Baysilon m350 0.5% Cetiol PGL 7.0% Myritol 312 3.0% Cetiol oe 4.0% Copherol 1250 0.5% PHASE 2 D-panthenol 1,0% Glycerin 86% 5.0% Aqua 71.5% PHASE 3 Carbopol 980 0.2% Cetiol PGL 1,0% PHASE 4 KOH 20% 0.3%

The speed of sound in multiphase media, such as cosmetic emulsions, does not differ much from the same value for water ((~ 1500 m / s), which allows us to calculate the optimal gap b for a channel at a given resonant frequency with sufficient accuracy. The wavelength is ~ 6.1-6.2 centimeters, respectively, for the superposition of waves inside the channel with in-phase generation of oscillations on the sides, and the small side of the rectangular profile should be ~ 1.55 centimeters (a quarter wave) or ~ 3.1 centimeters (half-wave resonator). specific second design uses the second option (half-wave).

The experiments showed that in practice the use of resonators with a small resonator side exceeding the wavelength leads to a sharp deterioration in energy characteristics. Therefore, in practice, the number k a, apparently, will not exceed the number 4 (wavelength).

When preparing the emulsion, three stages were distinguished:

- heating and preparation of the base (base);

- base cooling stage;

- the introduction of active additives and perfumes at a temperature of 40-45 ° C and homogenization at a constant temperature.

At stages 1 and 3, respectively, different oscillation amplitudes were set, at stage 2 (cooling), the cavitation mode was turned off, while at stages 1 and 3 the cavitation threshold was exceeded, but the intensity at stage 3 was approximately 4 times lower than at stage 1. These modes are controlled by thermal measurements at the input and output of the channel and by the indicator of the power supplied to the piezoelectric emitters.

Figure 6 presents a photograph of the emulsion with digital processing filter "smart sharpness", obtained using this method of obtaining the emulsion on the same scale as the photographs of Figures 1 and 2. Figure 7 shows the differential size distribution of the dispersed phase for the prototype (MIRRA cream ) on a smaller scale than in Figure 3, one of the products of the world leader - the company L Oreal and distribution for the cream obtained by the proposed method. All products belong to the same class - daily moisturizing face creams (direct emulsions).

This texture of cosmetic emulsion for consumers gives a number of new properties:

- tactile and organoleptic characteristics significantly improve (ease of application and grinding, quickness of absorption, absence of a greasy film after application). Marketing research (panels) was conducted, where as a result of anonymous questioning, 87% of women and girls (65 respondents) chose cream as the "best" in terms of organoleptic characteristics, prepared according to the proposed method, in relation to a cream of a similar composition, but prepared using classical technology;

- to obtain a stable emulsion, it is enough to use only 30-40% of the emulsifier of the amount necessary for cooking according to the classical technology / 7 /. It is known that reducing the amount of emulsifier reduces the risks of destruction of the lipid barrier of the skin, i.e. contributes to the preservation of healthy skin;

- the resulting emulsion has a pronounced express effect. With constant use, after 5-7 days, dry skin disappears, even when washing dishes with known cleaning products, which was noted by the respondents.

Experiments show that the proposed method for producing emulsion cosmetic products allows you to:

- get a smaller size dispersed oil (fat) phase;

- get a high level of homogeneity of the emulsion.

LITERATURE

1. Chervyakov V.M., Only V.G. The use of hydrodynamic and cavitation phenomena in rotary devices. - M.: Publishing House Engineering, 2008.

2. Sirotyuk M.G. Experimental studies of ultrasonic cavitation. In the book: Powerful ultrasonic fields. / Ed. L.D. Rosenberg, 1968.

3. Krasilnikov V.A. Sound and ultrasonic waves in air, water and solids. - M .: Fizmatgiz, 1960.

4. Bergman L. Ultrasound and its application in science and technology. - M .: Foreign literature, 1956.

5. The newspaper "Mirra Lux". Section "Expert Conversation. Interview with the Chief Production Technologist". June 1999.

6. Emulsions and emulsion technology, ed. K.J. Lissant, pt 1-2, New York, 1974.

7. V.I. Demenko, A. A. Getalov, T. V. Puchkova, E. A. Hoteenkova. An effective method of reducing the content of emulsifier in the manufacture of cosmetic emulsions. - Magazine "Raw materials and packaging" No. 10 (101), p. 12.

8. Vibration in technology. Handbook in 6 volumes, ed. Chelomeya V.N., M., Mechanical Engineering, 1979.

Claims (1)

A method of obtaining an emulsion cosmetic product, which includes stepwise dispersion in a solvent at room temperature of poorly soluble components such as vegetable oil, emulsifier and biologically active substances of various origins, solid powdery ingredients (sorbents or abrasives), the components are introduced into the installation with powerful sonication, in which the dispersion of the components and the cavitation homogenization of the emulsion are carried out, followed by packaging, distinguishing In that the resonant acoustic cavitation mode is formed inside a flowing mechanical vibrational system of a channel of rectangular cross section with large side a and small side b, respectively, sound vibrations are generated in phase on both opposite sides a with an amplitude exceeding the acoustic cavitation threshold for a moving multiphase medium, consisting of mixed ingredients, and the amplitude of the vibrations is selected optimal for the various stages of preparation of the emulsion, and the frequency f s ukovyh oscillations selected to equal the resonant frequency of all channel elements associated mass as determined by any known method, the minimal distance b between the walls of the channel selected multiple of a quarter wavelength, is excited in the multiphase medium:
b = (k / 4) · (C / f), k = 1,2,3, ...,
where f is the frequency of the generated oscillations, Hz;
C is the speed of sound in a multiphase medium, m / s;
b is the distance between the walls of the channel, m

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