Untitled record

FRENCH REPUBLIC

MINISTRY

INDUSTRY AND TRADE

PATENT

INDUSTRIAL PROPERTY SERVICE

Gr. 14. - CI. 6.

NOT^u 1.007.282

Improvements in methods and devices for obtaining gaseous emulsions, such as foams, from a liquid, viscous or pasty medium.

Mr. Jacques-Jean ESTIGNARD-BLUARD residing in France (Seine).

Requested March 15, 1948, at 16 ”4 ', in Paris.

Issued February 6, 1952. - Published May 5, 1952.

(Patent of invention whose del ivery was deferred in execution of article 11, § 7, of the law of July 5, 1844 modified by the law of April 7, 1902.)

The present invention relates to methods and devices for obtaining gaseous emulsions, more especially foams, from a liquid, viscous or pasty medium, hereinafter called "liquid medium" and which is generally aqueous.

It aims, above all, to make these processes and devices such that gaseous emulsions or foams can be obtained in a simple and economical manner, in desired quantities and at the times when desired, from an easily renewable reserve. .

It consists, mainly, - with regard to the processes of the kind in question - in bringing together, in an enclosed space, the liquid medium, which one wishes to transform into foam, and a liquefied gas, that is to say say which is in the liquid state when it is brought into contact with said thick medium but which becomes gaseous at the pressure and temperature conditions to be considered for its final state, and to deliver the whole by throttling in an atmosphere, especially the open air, in which there prevails a pressure lower than that of said enclosed space, so that the liquefied gas can spontaneously relax to form, with said liquid medium, the gaseous emulsion which it is desired to obtain;

And - with regard to devices of the kind in question - to constitute them by a container capable of receiving both the liquid medium and at least one liquefied gas which is practically insoluble in said medium but which spontaneously transforms into a gas with pressure and temperature conditions to be considered for its final state, said container comprising a nozzle by which the liquid medium and the liquefied gas can be expelled simultaneously, under the control of a shutter, by the effect of the vapor pressure of said gas to form at the outlet 2 - 41032

Booklet price: 100 francs.

said nozzle, with the entrained and discharged liquid medium, the gaseous emulsion which it is desired to obtain.

The invention consists, apart from this main arrangement, of certain other arrangements which are preferably used at the same time and which will be more explicitly discussed below, in particular:

In another provision, consisting in adding to the liquefied gas, used for the production of emulsions of the kind in question, an auxiliary product capable of diluting the liquefied gas, reducing its flammability and / or increasing the pressure, prevailing in space enclosed that contains it;

And in another arrangement, consisting of delivering the gaseous emulsion into an intermediate space in which it is brought into contact with a material of a different nature, which may be another gaseous emulsion, so that it can react with it before reaching its final state.

It relates more particularly to certain modes of application as well as certain embodiments of said provisions; and it relates more particularly still, and this as new industrial products, the gaseous emulsions obtained by the processes comprising application of said provisions, the devices, apparatus and installations suitable for the implementation of these processes, as well as the elements, tools and spare and replacement parts (bottles, flasks or reserve containers), used to build these devices.

And it can, in any case, be well understood with the aid of the additional description which follows as well as of the appended drawing, which description and drawing are, of course, given above all by way of indication.

Figs. there 3 of this drawing show, in section

Original ADB û [U 107.-2821 - i schematic axial, respectively three different hispo 'sitives established in accordance with the invention.

According to the invention and more particularly according to that of its modes of application as well as those of the embodiments of its parts to which it seems that there is reason to give preference, proposing to prepare a gaseous emulsion with using a liquid, viscous or pasty medium and a gas. we take it as follows or in analogous fashion.

The liquid, viscous or pasty medium used can consist of solutions, pastes, gels, suspensions, etc., preferably in an aqueous vehicle or support. The emulsifying products which are found in this medium can be salts of fatty and naphthenic acids, sulfonates, salts of acid sulfuric esters of fatty alcohols, these salts being obtained by the action of alkaline bases or ainines (ethanolamines) , certain fatty amines, so-called inverted soaps, emulsifiers derived from ethylene oxide and di-ethylene glycol, lecithin, etc.

These liquid media can be used separately or in combination in any desired proportion.

The liquefied gas, which is placed in the presence of the aforementioned liquid medium, in a closed space or vessel, is chosen so that it is inert or indifferent to the substances constituting this medium, that it is liquefiable at ordinary temperature and at a relatively low pressure, that it practically does not dissolve these substances or that it is insoluble in them but that it can form with them a liquid and uniform emulsion, of the “oil in water” type, as long as the gas remains in the liquid state. On the other hand, this liquefied gas returns to its gaseous state at the operating pressure (atmospheric) for a temperature zone of between approximately - 50 ° C and + 30 ° C.

To obtain this liquefied gas, recourse may be had to saturated, unsaturated or cyclic hydrocarbons with 3, 4 or even 5 carbon atoms, monochlorinated or monobrominated derivatives of methane, ethane and ethylene, certain fluorinated derivatives and fluorochldrees of methane and ethane, methyl or ethyl nitrite and, more particularly because of their industrial importance, butanes and butylenes, stabilized butadiene, propane, propylene, monomeric and stabilized vinyl chloride, methyl bromide, ethyl chloride, ledichloro-difluoromethane, monochloro-tetrafluoroethane, dichloro-monofluoro-methane, trichloro-monofluoromethane, and many others.

The liquefied g iz specified above. can also be used separately or in combination in any proportions.

In some cases or may also use carbon dioxide, compressed air, etc., in conjunction with one or more of the liquefied gases indicated above, in particular to dilute them, to reduce their immobility or to increase the pressure in the space or closed cup.

The liquid medium may also contain fine particles or suspended solid fillers as well as stabilizers and / or thickeners, in particular colloids such as alkaline alginates, ag.ir-agar, arabic gums, adraginte, glues, proteins or albumins degraded or not, aluminum gels or iron hydroxide, etc.

The liquid medium and the liquefied gas can be emulsified beforehand and by known means, with or without the addition of CO, auxiliary and / or stabilizers or thickeners. in suitable and desired proportions in airtight containers in pressure or in the open air but at a temperature such that the vaporization is practically zero. A liquid emulsion is thus obtained which is stored in bulk in a closed container and which can be distributed, in desired quantities, in containers, flasks, bottles, etc., which are sufficiently resistant to pressure and which are used for use. The initial liquid emulsion can also be dispensed directly by a nozzle, a gun or the like without first transferring it into one or more auxiliary receptacles.

It is also possible to prepare a specific charge for a container or flask, serving for use, and to introduce therein first one of the essential constituents (liquid medium or liquefied gas) and then the other.

It is also possible to fill a container or flask with the liquid medium only and to introduce therein, after the fact and at the desired time, the liquefied gas to obtain the liquid emulsion.

Whatever the mode of preparation adopted, the liquid emulsion is stored or collected in a closed space resistant to the pressure to be considered and it is delivered by at least one nozzle (nozzle, nozzle, gun, etc.) que.l 'We put in communication with this space by the opening, more or less large, of a shutter (tap, valve, valve, needle, etc.) operable from the outside. The expulsion of the liquid emulsion, out of this space, is done automatically by the effect of the vapor pressure of the liquefied gas and the nozzle delivers, finally, a foam obtained by the spontaneous vaporization 'bad ORIGINAL of the liquefied gas , the flow rate of this foam depends in particular on the nature of the substances used, the pressure prevailing in the closed space and the degree of opening of the shutter while its volume and its consistency depend on the relative proportions of the ingredients forming this liquid emulsion .

Liquefied gas forms one of the essential constituents of the liquid emulsion, which is the intermediate product from which the gas or foam emulsion is obtained in the end, and also provides the pressure by which the expulsion of this emulsion is obtained. liquid.

Instead of using a single device with one or more debit nozzles, it is possible to combine at least two of these devices to bring into contact or in contact with different gaseous emulsions or foams capable of reacting chemically with each other, by example a polymerizable resin and a polymerizing repellant as in the case of a foaming glue preparation or a rubbery and spongy product.

The invention is therefore based on the observation made by the inventor that most substances capable of emulsifying liquids in a given medium are also suitable for emulsifying a gas in this same medium. It should be noted that the vapor pressure of the liquid emulsion thus obtained is independent, within wide limits, of the relative proportions of the liquid medium and of the liquefied gas and that it corresponds_vpractically at the vapor pressure of this gas at the pressure and temperature conditions to be considered. As a result, it is possible to obtain gaseous or foam emulsions, having variable consistencies and volumes and containing different proportions of gas, by simply varying the quantity of the liquefied gas contained in the initial liquid emulsion. Generally, proportions of 10 to 20% of the liquefied gas, relative to the liquid medium, give good results without these values ​​having a restrictive or limiting meaning. It is thus possible to obtain a foam containing an amount as reduced as 1% of the liquid medium, the remainder being formed by expanded gas so that the volume of the foam corresponds substantially to that of this gas. . It is thus possible, for example, to easily obtain a volume of 100 liters of foam from a liquid emulsion corresponding to approximately one liter.

The process which is the subject of the invention therefore clearly differs from the usual methods by which gaseous emulsions are prepared, for example those by which a compressed gas is dissolved by stirring or injection into a liquid (mineral water), those by the [1.007.2821! which of the pulverulent, clean materials 3 I give off gases. at determined temperatures I are mixed with liquids (sparkling water) or pasty or viscous substances (spongy articles) because in all these cases the volume of the gaseous emulsion, obtained in the end, remains equal or becomes barely greater than that of the initial mass which served for the preparation.

The invention thus makes it possible to store under a reduced volume a preparation which provides a foam having an extremely large volume so that this preparation can be stored in a container having a small footprint and whose weight is hardly excessive since this container should only be able to withstand relatively low pressure (a few kg .cm¹). This container can therefore be portable and is, in any case, easy to handle. In addition, the intermediate liquid emulsion is obtained without significant stirring and without the addition of heat.

In the enclosed space (container, flask, etc.), which contains the liquid emulsion under pressure, there are at least three phases, one of which is a gaseous phase formed by the saturated vapor of the liquefied gas including, where applicable, that of CO 2 or the like in the presence, while the other two phases are more or less liquid, one being constituted by the liquid medium saturated with liquefied gas and the other by the liquefied gas saturated by said medium.

The gaseous emulsions obtained can be used for a variety of purposes, among which there may be mentioned, by way of example, soap-based products for the toilet and. beard, toothpaste, beauty creams, eyeshadows, hair care products, various maintenance or cleaning products (polishes, polishes), ointments, ointments, lubricants, fire extinguishing media, insulating, heat-insulating or sound-absorbing materials, colored foams for camouflage, polymerized foams for packaging, food products (meringues, egg yolks), rubber-based materials, natural or artificial and cellulosic materials for the manufacture of spongy articles or objects, foam adhesives, etc.

The process for producing foams or the like lends itself very well and for several uses to automatic dispensing, for example using a token device.

The appended drawing shows, by way of nonlimiting or restrictive examples, three different modes of re-use which are suitable for the characteristic features of the devices which are the subject of the invention.

We have admitted that we are using a container

BAD ORIGINAL L.

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[1.007.282] - or bottle 1. of reduced capacity and made of metal, glass or a plastic and removable material, sufficiently resistant, into which a predetermined quantity of the liquid emulsion prepared in advance or of the ingredients is introduced intended to form this emulsion. The neck 2 of this container is threaded or has other fixing means so that one can mount, on this neck and in a removable manner, a simple ordinary threaded plug, with or without dip tube, or a gasket, metal or any other suitable material, with a debtor nozzle 3 and with shutter means. This gasket preferably carries a dip tube 4, the open end of which ends near the bottom of the container.

For the example shown in fig. 1, it has been admitted that the container is filled at the place where the emulsion is prepared with the product ready for use, this preparation can, as indicated above, be carried out either in separate tanks or apparatus fed, intermittently, with successive or stationary charges, or continuously, with the ingredients necessary for the preparation of this emulsion. These devices include suitable dispensing means with the aid of which a large number of containers provided with linings similar to that shown in FIG. 1. Each container or bottle is thus supplied in full to the user and its lining remains permanently on the neck 2 and is removed, to allow a new filling, only by the manufacturer when the empty container is returned to him.

The packing, shown by way of example only in FIG. 1, comprises a · lateral nozzle 3, the axial passage 5 of which communicates with the open air through a calibrated orifice 6 while its internal end opens into a chamber 7 formed axially in the body 8, screwed onto the neck 2. The chamber 7 can communicate, through an orifice 9, with a cavity 10 formed in the lower part of the body 8 above a plug 11 which closes the container 1 and whose central orifice 12 serves as a housing at the end upper of the dip tube -1.

The edge of the orifice 9, established between the chamber 7 and 11 cavity 10, forms a conical seat for a valve 13, the rod 14 of which is secured to a cap 15 freely engaged on the upper end of the body 8. This cap I 5 can slide and rotate relative to said body and this movement is made possible by a slot or opening 16 made in the iterative wall 1 of the cap 15 and in which the nozzle 3 is engaged. This slit has the shape of an elongated S I so that the cap 15 can come to occupy | -

an extreme position for which the valve 13 is applied to its seat 9 by a spring 1 3 a. By rotating the cap 15 in the proper direction, it slides along the body 8, more or less opening the valve 13.

The liquid emulsion, contained in the container 1. can thus flow, by the pressure prevailing in the container, and will escape outside through the calibrated orifice 6 of the nozzle 3, spontaneously transforming into a gas emulsion. When the cap 15 is returned to its initial position, the valve 13 is applied to its seat and the flow of the emulsion is interrupted.

For the example shown in fig. 2, it is assumed that the container 1 is supplied to the user by the manufacturer without it having its obturating and distributing lining. In this case, a cover 17, made of a ductile metal, is applied to the upper part of the neck 2 of the container while being held in place by temporary fixing means, for example a ring 1 8 screwed onto the neck 2 of the container 1 , so that this seal covers the upper end of the tube 4.

The gasket is similar to that described above except that the underside of the valve 13 carries a tip 19 whose free end is opposite the central part of the cover 1 7 and can pierce it when the cap 15 is brought to its characteristic position for which the valve 13 is open. This piercing takes place once and for all before the container is put into service and when the cover 17 has been crossed by the tip 19, the device operates as that described with the aid of FIG. 1.

When the container is empty, the user unscrews the filling to fix it on a new full bottle.

For · the example shown in fig. 3, it is assumed that the container 1 contains only a predetermined quantity of the liquid medium and that the liquefied gas is introduced after the fact by auxiliary and removable means, comprising a sleeve 21 screwed onto the threaded neck 20 of the container 1 on the threaded end 22 from which a socket 23 is engaged which serves as a support for the plug 11 carrying the dip tube 4 and on which a packing similar to that shown in FIG. 1.

On the internal face of the side wall of the sleeve 21 an annular part 27 defining an opening 24 is mounted, this part forming a seat for a valve 25 the external face of which carries a central point 26, engaged in a hole 28 provided in the side wall of the sleeve 21 opposite the opening 24. On either side of this hole are established ears 5 to which a removable stirrup 30 is articulated, the crosspiece of which carries a threaded rod 31 provided with a button operating 32.

In this stirrup one can engage a metallic bottle 33. similar to those which are used to load with carbon dioxide the bottles of Selz water. This bottle contains the liquefied gas and its neck is closed by a pellet, made of a ductile metal, which can be pierced by the tip 26 of the valve so that its content can automatically penetrate into the container 1, through 25 ° orifices made in the valve, these holes being closed when the valve is applied to the edge of the hole 28 when, after emptying the bottle, it is removed by releasing the valve. This then closes the hole 28 and the device is ready to operate in a manner analogous to that explained with the aid of FIG. 1.

As a result, a process and a device are obtained for preparing a gaseous or foam emulsion which responds well to the aims which it has been proposed to achieve, this preparation being carried out using simple, light, robust means. and space-saving. In addition, by a judicious choice of the proportions of the ingredients, which one uses to obtain this emulsion, one can vary, at will, the physical characteristics (volume, consistency, dry matter content, gas content, etc. .) in each particular case.

As is obvious and as already follows from the above, the invention is in no way limited to that of its modes of application any more than to those of the embodiments of its various parts, having been more specially indicated ; on the contrary, it embraced all the variants.