FR2660212A1 - Process for the preparation of an emulsion and emulsifiable composition - Google Patents

Abstract

The oily and aqueous constituents of an emulsion to be prepared are stored separately from one another in a receptacle. The oily constituent is enclosed in multiple capsules made of a mixture of agar gel, an agent for destroying the capsules and purified water, and floating in the aqueous constituent. The capsules are broken and the oily constituent leaving the broken capsules is mixed with the aqueous constituent to form an emulsion a little at a time, each time the need becomes apparent. The broken capsules are divided by the agent for destroying the capsules into fine particles dispersed in the emulsion.

Description

PROCESS FOR THE PREPARATION OF AN EMULSION AND COMPOSITION
EMULSIBLE
This invention relates to an emulsified cosmetic or non-medicinal preparation, such as a cream or a lotion.

 An emulsified cosmetic or non-medicinal preparation is known which mainly comprises an oily constituent such as a fatty acid, an oil or a fatty substance, or else a wax, an aqueous constituent such as a humidifier or purified water, a surfactant which promotes emulsification and a dispersion of one of these constituents in the other, and an antioxidant for the oily constituent.

 It is an emulsion prepared by heating a well-proportioned mixture of these substances and contained in a container.

 The surfactant is essential to stabilize the quality of the preparation. The proportion of surfactant in the mixture has a decisive impact on the quality of a lotion type product in particular.

The antioxidant prevents the lowering of the quality of the preparation which is likely to cause the oxidation of its oily component by exposure to air, ultraviolet rays, etc.

 Until now, it was essential, for any emulsified cosmetic or non-medicinal preparation, that it contains both the surfactant and the antioxidant, because it would otherwise suffer a great drop in quality during its storage due to the separation of its oily component from its aqueous component or to the deterioration of its oily component by oxidation.

The use of a surfactant or an antioxidant in a cosmetic preparation or the like should however be avoided as much as possible, since neither is very good for the skin.

 Under these circumstances, an object of this invention is to provide a process which can minimize, or even eliminate, the addition of a surfactant or an antioxidant to a cosmetic or non-medicinal emulsion of the type which does not require elimination by washing. on the skin once applied, such as a cream or lotion, so that the emulsion cannot cause damage to the skin, and which nevertheless makes it possible to prepare a high quality emulsion, when it is necessary to apply it on the skin.

 Another object of this invention is to provide an emulsifiable composition which can form a high quality cosmetic or non-medicinal emulsion which does not cause any damage to the skin, when it is necessary to apply it to the skin.

 These goals are achieved primarily by a process which includes the steps of keeping the oily and aqueous constituents of an emulsion separate from each other and mixing them to form an emulsion immediately before 'employment, and thanks to an emulsifiable composition which comprises maintaining the oily and aqueous constituents separately from each other until they are mixed to form an emulsion immediately before use.

 The first aspect of this invention relates to a process for the preparation of an emulsion which comprises the steps which consist in keeping the oily and aqueous constituents of an emulsion, the constituent separately, in a container, separately from one another. oily being enclosed in multiple capsules formed from a mixture of agar, a capsule destructing agent and purified water and floating in the aqueous component, and breaking the capsules to mix the oily component and the component aqueous, to form an emulsion immediately before use, the agar being destroyed by the capsule destroying agent to form fine particles dispersed in the emulsion.

 The second aspect of this invention relates to an emulsifiable composition which comprises an oily component enclosed in multiple capsules and an aqueous component contained in a container, the capsules floating in the aqueous component.

 The third aspect of this invention relates to an emulsion preparation device, which comprises a container for containing an aqueous component of an emulsion and an oily component enclosed in multiple capsules floating in the aqueous component, and a mechanism provided in the container for breaking the capsules in order to mix the oily component and the aqueous component to form an emulsion and to push the emulsion out of the container.

 Other objects, characteristics and advantages of this invention will appear on reading the description which follows and the accompanying drawings.

 Figure 1 is a longitudinal sectional view of a device which can be used to implement a method according to this invention and which contains an emulsification mechanism located in the upper position.

 Figure 2 is a view similar to Figure 1, but which shows the device in which the emulsification mechanism is located in the low position.

 FIG. 3 is an enlarged view of the emulsification mechanism in substantially the same position as in FIG. 2.

 Figure 4 is a view similar to that of Figure 3, but showing the mechanism in substantially the same position as in Figure I.

 Finally, Figure 5 is a longitudinal sectional view of a modified form of the device that can be used to implement the method of this invention.

 Referring to Figure 1 of the drawings, there is shown a device enclosing a container containing an emulsifiable composition used to form a cosmetic or non-medicinal emulsion. The composition comprises an oily component 2 and an aqueous component 4. The oily component 2 is stored in multiple capsules 1 made mainly of agar. Each capsule 1 and the oily constituent 2 which it contains defines an encapsulated unit 3 of the oily constituent 2. The encapsulated units 3 normally float in the aqueous constituent 4 within the container 5. The container 5 is provided with a mechanism 6 serving to break the capsules 1, to mix the oily and aqueous constituents 2 and 4 and to form an instantaneous emulsion, and to push it out of the container 5.

 The capsules 1 are formed from a material which is prepared by dissolving agar and a thickening agent in purified hot water, adding a pulverulent pigment, and mixing them carefully. Agar is the main substance in capsules I and serves to protect the oily component 2 from the aqueous component 4 and to keep it stable. The thickening agent is an auxiliary which is added to regulate the mechanical resistance of the agar membrane defining each capsule 1. For example, sodium alginate is used as a thickening agent.

 The powdery pigment is added as a destroyer of the capsules to promote fine division and dispersion of the agar membranes when the capsules 1 are ruptured, until no large unwanted agar particles remain. For example, as powdered pigment, la-sericite, micaceous titanium or titanium dioxide is used. It is also possible to use a cosmetic powder pigment, such as talc or calcium oxide.

 The oily constituent 2 consists of an oil or a fatty material, such as squalane or jojoba oil, a fatty acid such as stearic acid or myristic acid, a neutral fatty acid such as glyceryl trioctanoate, an emulsification aid, such as cholesterol hy droxystearate or lecithin, which may be added, and other additives such as natural vitamin E, and a perfume. Neutral fatty acid is added as a density regulating agent to adjust the density of the oily component 2 in the range of 9.0 to 9.8, so that the encapsulated units 3 can always float in the aqueous component 4 .

 One can, for example, prepare each encapsulated unit 3 by placing a double-walled nozzle in a cooling liquid, by injecting the oily component 2 into its internal cylinder and a mixture of the materials of the capsules in the gap between its internal and external cylinders. , both in the heated and molten state, and by applying an ultrasonic vibration to the nozzle, which makes it possible to form spheres of the capsule materials to form a capsule 1 defining an empty space in which the oily component 2 is enclosed. Each encapsulated unit 3 is a ball having a diameter close to 3 mm. The capsule 1 can occupy 30 to 90% by weight of the unit 3. The unit 3 preferably consists of 70% by weight of capsule 1 and 30% by weight of oily constituent 2.

 The aqueous component 4 is prepared by dissolving a thickening agent, such as a carboxyvinyl polymer, in purified water, to form an aqueous solution, by mixing a viscosity modifier, such as sodium hydroxide, in the solution for neutralize, and adding other additives, such as a humidifier, to the solution.

The additives are a humidifier, such as concentrated glycerin or dipropylene glycol, a natural high molecular weight humidifier such as atherocollagen or biohyaluronic acid, a buffering agent such as sodium citrate, a preservative such as alcohol and a preservative. - a carrier such as a para-hydroxybenzoic ester or phenoxyethyl alcohol.

 The container 5 can contain the encapsulated units 3 and the aqueous component 4 at a rate of, for example, 50% of each. The encapsulated units 3 float in the upper part of the aqueous component 4, because they have a density of 9.0 to 9.8, which is regulated by the density regulating agent.

 The device will now be described in more detail with the aid of FIGS. 1 to 4. The container 5 is essentially a cylinder formed of glass or of a hard synthetic resin and the top and bottom of which are open. The cylinder preferably has a transparent or semi-transparent wall, making it possible to see the quantity of its content which remains.

The lower opening of the container 5 is closed by a sliding shutter 7 made of a flexible material, such as synthetic rubber, and by a detachable cap 8.

The shutter 7 has a double cylinder construction and encloses an external cylinder comprising a pair of annular sliding parts 7a and 7b, protruding respectively from its lower end and from its upper end, and kept in sliding contact with the surface of the internal wall. of the container 5, and an internal cylinder in which the plug 8 is mounted. The bottom of the container 5 is further capped with a protective capsule 9.

 The mechanism 6 used to break the capsules, to mix the oily and aqueous constituents to form an emulsion and to push it out of the container, which will hereinafter be called the emulsification mechanism, is mounted in the upper opening of the container. 5. The emulsification mechanism 6 comprises a guide cylinder 10 and a suction cylinder 11, which are fixed elements, a sliding rod 12, a valve cylinder 13, a push cylinder 14 and an actuating capsule 15, which are movable elements, and a ball 16 defining a non-return valve, a coil spring 17, a packing element 18 and a retaining ring 19, which are intermediate elements.

 The container 5 has a neck surrounding its upper opening. The guide cylinder 10 has a double wall cylindrical construction. The packing element 18 is annular and is placed between the upper end of the container neck 5 and the lower end of the outer cylindrical wall part of the guide cylinder 10. The retaining ring 19 is mounted around the upper end of the neck of the container 5 and of the lower end of the outer cylindrical wall part of the guide cylinder 10 to hold them, as well as the lining element 18, in a liquid-tight manner.

 The suction cylinder 11 has a number of annular shoulders at the level of which its internal diameter and its external diameter decrease in a staggered manner from its upper end to its lower end. It has an upper end portion disposed between the outer and inner cylindrical wall portions of the guide cylinder 10, and its upper end is held against the inner surface of the annular upper end of the guide cylinder 10 which connects its cylindrical wall portion outer and its inner cylindrical wall portion. The suction cylinder 11 has a middle part which contains the non-return valve or ball 16. The ball 16, which is made, for example, of stainless steel or a hard synthetic resin, is free to move in a certain axial measurement with respect to the suction cylinder 11.

 The push cylinder 14 consists of a top part and a bottom part whose diameter is larger than that of the upper part. Its lower part is arranged movably vertically in the internal cylindrical wall part of the guide cylinder 10 and has a bottom which can be coupled with the guide cylinder 10, so that the push cylinder 14 can stop any other movement towards the low. The sliding rod 12 has an annular flange 12a projecting radially from its middle part. The rod 12 has an upper part situated above the flange 12a and the peripheral surface of which is formed by several longitudinal grooves 12b, which extends into the lower part of the push cylinder 14.The coil spring 17 surrounds the lower part of the rod sliding 12 located below the flange 12a and has an upper end held against the flange 12a and a lower end held against a shoulder formed on the inner wall surface of the middle portion of the suction cylinder 11. This is what which allows the spring 17 to normally push the sliding rod 12 upwards.

 The valve cylinder 13 is made of a flexible synthetic resin and essentially surrounds the middle part of the sliding rod 12. The valve cylinder 13 has an upper end fixed to the bottom of the push cylinder 14 and a lower end whose outer surface is maintained in sliding contact with the internal wall surface of the suction cylinder 11. The actuating capsule 15 has an essentially cylindrical double wall construction and has an internal cylindrical wall part in which is fixed the upper part of the push cylinder 14 and an external cylindrical wall part surrounding the guide cylinder 10. The guide cylinder 10 has its upper part disposed between the internal cylindrical wall part and the external cylindrical wall part of the actuating capsule 15, so that the capsule 15 can slide vertically along the guide cylinder 10. The internal cylindrical wall part of the c apsule 15 has an axial bore which ends in a nozzle 15a directed horizontally.

 The plug 8 is detachable from the obturator 7 to allow filling of the container 5 with the encapsulated units 3 and the aqueous component 4. It is possible to eliminate or minimize the addition of antioxidant to the encapsulated units 3, because the capsules 1, made mainly of agar, protect the oily component 2 from oxidation. In addition, it is possible to eliminate or minimize the addition of surfactant, since the oily and aqueous constituents 2 and 4 are not mixed until the emulsion is needed.

 The emulsification mechanism 6 normally remains in the high position, as indicated in FIG. 1, because the coil spring 17 pushes up the sliding rod 12 and therefore the push cylinder 14 and the capsule 15. If one applies appropriate finger pressure in the direction of arrow A in FIG. 1 to lower the capsule 15, the push cylinder 14 is moved downwards to press on the sliding rod 12 overcoming the force of the spring 17, which means that the mechanism 6 as a whole is lowered to the low position as shown in FIG. 2. As soon as the finger pressure is stopped, the mechanism 6 returns in the direction of the arrow B in FIG. 2 and the mechanism 6 as a whole returns to the high position as indicated in FIG. 1.

 When the mechanism 6 remains in the high position, the internal and external surfaces of the valve cylinder 13, adjacent to its lower end, are kept in intimate contact with the peripheral surface of the annular flange 12a of the sliding rod 12 and of the internal surface. of the suction cylinder 11, respectively, and the suction cylinder 11 defines a storage compartment 20 surrounding the lower part of the rod 12. The storage compartment 20 already contains the encapsulated units 3 and the aqueous component 4 which have been sucked into the suction cylinder 11, as will be described in more detail below. If the emulsification mechanism 6 is lowered to the low position, the encapsulated units 3 and the aqueous component 4 located in the storage compartment 20 are progressively compressed, as the ball 16 is lowered and closes the storage compartment 20 at the bottom. When the mechanism 6 arrives in the low position, the lower end of the valve cylinder 13 abuts on a shoulder formed on the internal surface of the suction cylinder 11 and the internal surface of the valve cylinder 13 is separated from the annular flange 12a of the sliding rod 12, which forms a gap between them making it possible to establish a fluid communication between the upper part and the lower part of the sliding rod 12, as shown in FIG. 3. This results in the flow of the compressed mass of the encapsulated units 3 and of the aqueous component 4 outside the storage compartment 20. When this flow occurs, the capsules 1 are ruptured by the coil spring 17 and the oily component 2 mixes with the aqueous component 4 to form an emulsion. The resulting fragments of capsules 1 are finely divided by the pulverulent pigment used as agent for destroying the capsules and dispersed in the emulsion.

The emulsion which has been formed in the longitudinal grooves 12b of the sliding rod 12 and the axial bore of the pusher cylinder 14 is expelled in the form of a jet by the nozzle 15a of the capsule 15.

 If the finger pressure on the capsule 15 is stopped, the emulsification mechanism 6 returns to the high position under the action of the coil spring 17. The valve cylinder 13 contracts diametrically and enters again. intimate contact with the annular flange 12a of the sliding rod 12, as shown in FIG. 4. The negative pressure which has been created in the storage compartment 20 means that an additional quantity of the encapsulated units 3 and of the aqueous component 4 is sucked into the storage compartment 20 by the suction cylinder 11, while pushing the ball 16 upward and flowing at its level. When the encapsulated units 3 and the aqueous component 4 flow at the spring with flange 17, the capsules 1 are ruptured by the spring 17 and the oily component 2 leaving the ruptured capsules mixes with the aqueous component 4 to form an emulsion. The ruptured capsules are finely divided and dispersed in the emulsion, because the powdery pigment added to the capsule material as an agent for destroying the capsules promotes the destruction of the agar molecules.

 When the emulsification mechanism 6 is returned to the high position, the storage compartment 20 therefore maintains the emulsion in its upper part outside the coil spring 17 and the oily component 2 encapsulated and the aqueous component 4 in its lower part. The emulsion is expelled in the form of a jet if the mechanism 6 is lowered again.

 The shutter 7 does not have the sole function of preventing leaks from the encapsulated units 3 and from the aqueous component 4 due to its annular sliding parts 7a and 7b which maintain intimate contact with the internal surface of the container 5. When the content of container 5 decreases, the shutter 7 is pushed up from time to time, as indicated by arrow C in FIG. 2, to facilitate the transfer of the encapsulated units 3 and of the aqueous component 4 from the container 5 to the emulsification mechanism 6.

 A modified form of the device is shown in FIG. 5. It comprises a container 21 formed from a tube of flexible synthetic resin. The container 21 has a neck, a diametrically enlarged part of which defines a storage compartment 22. The storage compartment 22 contains a non-return valve, or ball 23, at its inlet and is provided, at its outlet, with a fine grid. cylindrical 25 serving to break the encapsulated units 3. A capsule 24 covers the upper end of the neck.

 The following presents a list which gives, by way of example, the respective formulations of a capsule, of an encapsulated oily constituent and of an emulsifiable composition for a cosmetic preparation of this invention, all in% by weight.

Caspules:
Purified water 88.00
Agar (main material) 1.50
Sodium alginate (manufacturing aid for
capsules) 1.50
Sericite (powdery pigment) 4.00
Micaceous titanium (powdery pigment) 2.50
Titanium dioxide (powdered pigment) 2.50
Encased oily constituent
Glyceryl trioctanoate (regulatory agent
density) 49.67
Jojoba oil (main oily substance) 30.00
Squalane (main oily substance) 20.00
Cholesteryl hydroxystearate (auxiliary
emulsification) 0.10
Stearyl glycyrrhetinate (anti-inflammatory) 0.05
Natural vitamin E (natural antioxidant) 0.05
Para-hydroxybenzoic ester (preservative) 0.03
Perfume 0.10
Emulsifiable composition
Encapsulated units (capsules and
encapsulated oily constituent) 50.00
Purified water 43,055
Carboxyvinyl polymer (thickening agent) 0.100
Sodium hydroxide (viscosity modifier) 0.025
Concentrated glycerin (humidifier) 2,500
Dipropylene glycol (humidifier) 2,500
Atherocollagen (natural humidifier of
high molecular weight) 0.100
Biohyaluronic acid (natural moisturizer of
high molecular weight) 0.100
Sodium citrate (buffering agent) 0.010
Alcohol (storage aid) 1,500
Para-hydroxybenzoic ester (preservative) 0.060
Phenoxyethyl alcohol (preservative) 0.050
As shown in the description above, it is sufficient that the emulsifiable composition for cosmetic preparation or non-medicinal preparation according to this invention contains only a very small amount of antioxidant, if at all, compared to the known emulsified preparations in the prior art, insofar as the capsules, mainly made of agar, contain the oily constituent and thus protect it from oxidation.

 Since the capsules are ruptured to allow the oily component to be mixed with the aqueous component to form an emulsion immediately before use, it is possible to eliminate or minimize the addition of surfactant which was essential in known preparations stored in the form of an emulsion.

 This invention therefore provides a high quality emulsified cosmetic or non-medicinal preparation which is safe for the skin. When the broken capsules are finely divided and dispersed by the capsule destroying agent, a smooth emulsion is obtained which can be applied to the skin only. It provides a very useful cosmetic or emulsified cosmetic preparation of the type which is not removed from the skin by washing after application, such as a cream or a lotion. The preparation can be applied easily and quickly to the skin, since the ruptured capsules are so finely divided and dispersed by the agent for destroying the capsules that there can be no agar particles left, for example, requiring wiping or washing skin.

 The invention has been described with reference to its preferred embodiments and it is understood that the above description is not intended to limit the scope of this invention, but that the ordinary person skilled in the art can easily make variations on it and modifications without departing from the scope of this invention, defined in the appended claims.

Claims (6)

1. Method for preparing an emulsion, characterized in that it comprises the steps which consist in  encapsulating an oily component in multiple capsules formed from a mixture of agar, capsule destroying agent and purified water;  filling a container with the encapsulated oily component and an aqueous component, the capsules floating in the aqueous component; and  applying pressure on part of the capsules and of the aqueous component to break the capsules and causing the oily component leaving the ruptured capsules to mix with the aqueous component to form an emulsion, the ruptured capsules being simultaneously divided into fine particles by the destruction of capsules. 2. Method according to claim 1, characterized in that the agent for destroying the capsules promotes the dispersion of fine particles in the emulsion. 3. Method according to claim 1, characterized in that the agent for destroying the capsules is a pulverulent pigment chosen from the group consisting of sericite, micaceous titanium, titanium dioxide, talc and calcium oxide. 4. Method according to claim 1, characterized in that the container is provided with a mechanism serving to break the capsules and to effect the mixing of the oily and aqueous constituents. 5. Emulsifiable composition used to manufacture a preparation applicable to the skin, characterized in that it comprises  an oily constituent enclosed in multiple capsules formed from a mixture of agar, a capsule destroying agent and purified water; and  an aqueous component, the capsules and the aqueous component being stored in a container, within which the capsules float in the aqueous component, until little by little material is used until the capsules are broken and the oily component leaving the ruptured capsules is mixed with the aqueous component to form an emulsion.  6. Composition according to claim 5, characterized in that the agent for destroying the capsules is a pulverulent pigment chosen from the group consisting of sericite, micaceous titanium, titanium dioxide, talc and calcium oxide.