BE825867A - COMPOSITE BODY OF MOLECULAR SIEVES FOR THE CARBONATION OF AQUEOUS BEVERAGES AND DEVICE INCLUDING SUCH A BODY - Google Patents

Description

       

  "Composite body of molecular sieves for gasification of aqueous beverages and device

  
including such a body "<EMI ID = 1.1>

  
absorbed. Carbon dioxide is released from molecular sieves by displacement through the water from the aqueous beverage. The released carbon dioxide dissolves in it to gasify it. The molecular sieves are bonded into a monolithic structure having a sufficient specific surface area for contact between the carbonated beverage to be carbonated and the molecular tanis, so that the carbon dioxide is easily displaced by the drinking water.

  
The industrial gasification of beverages generally indicates the contacting of carbon dioxide and liquid, under pressure and with intense agitation, in a cooled vessel. This industrial process obviously requires elaborate and complex equipment which is not available in the places where the drinks are consumed.

  
Various simple gasification processes have already been proposed, suitable for domestic use. Most often, these procedures

  
previous gasification methods involve the use of a chemical "couple" to form carbon dioxide in situ at

  
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Born by the combination of an inorganic carbonate, such as sodium bicarbonate, and an edible acid, such as citric acid or an acid-functional ion exchange resin. Contacting such compounds in an aqueous solution causes the formation of carbon dioxide and the salt of the edible acid. Several patents describe in detail certain preferred forms of such acid-bicarbonate or acid-bicarbonate resin combinations.

  
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quent the formation of organic salts in solution, which give

  
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se complex ions to prevent them from dissolving in the drink. The presence of such salts is particularly sensitive and unpleasant to the consumer when the formation is induced.

  
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use from dry drink compositions containing carbon dioxide which, in aqueous solution, react

  
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US 3,441,417). However, these compositions are quite complex and it is often necessary to incorporate a buffering system into the beverage solution.

  
Thus, it is proposed in patent BE 791 754 to carbonate aqueous drinks at the point of consumption using an effective amount of molecular sieves based on crystalline aluminosilicates having adsorbed at least 5% by weight of carbon dioxide. . Molecular sieves of the type used for carbonating beverages at the point of consumption are crystalline aluminosilicates of the general formula:

  
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in the form of salts, M being a metal cation, usually

  
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bre of moles of alumina and b the number of moles of hydrated water

  
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After removing at least a portion of the water of hydration by heating or "cooking", the crystalline aluminosilicates become highly porous and exhibit a multiplicity of surface cavities and internal pores defining in the crystal a network of communicating passages. As used in the present description, the term "cooking" denotes heating in an oven or by other suitable means in order to remove at least partially the water of hydration from the substances treated, but absolutely without vitrification of the substance. these substances.

  
Such dehydrated molecular sieves are said to be "activated" which

  
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carbon dioxide or other molecules capable of being adsorbed. Due to their crystalline nature, surface cavities and pores have very substantially uniform diameters.

  
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crystalline silicates have a wide field of application

  
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molecular sieves causes the drawbacks inherent in the use of small particles. Since these aggregates are not intended to be swallowed with the beverage, they must be surrounded by a casing or the like to easily separate them from the liquid beverage upon consumption. The various types of such casings for molecular sieve aggregates have economic, aesthetic or other disadvantages which may preclude their use for commercial purposes. By reu

  
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a good number of the drawbacks inherent in the use of a multiplicity of small aggregates would be eliminated. However, the realization of a suitable monolithic structure raises serious technological problems. A solid disc or tablet

  
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silicates joined together by a clay-based mineral binder is hardly satisfactory because of the difficulties raised by its use for the carbonation of liquid drinks; in order to obtain a ga-

  
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obtain a sufficient quantity of CO2 released in the drink and

  
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is maintained in the gasified state, the molecular sieves must adsorb at least a certain amount of CO2. Cr, when we place-

  
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liquid drink, the pressure generated by the carbon dioxide released from molecular sieves is often strong enough to disintegrate or destroy the disc. If we take steps to

  
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also unacceptable gasification times.

  
Accordingly, the present invention relates to a composite and rigid body of molecular sieves capable, after adsorption of an effective amount of carbon dioxide, of suitably carbonating an aqueous beverage without being destroyed or dissolved. It also relates to molecular sieve discs or pellets joined together by a binder, capable of effectively carbonating a drink for an industrially acceptable time. The invention also relates to simple but effective devices for the carbonation of beverages at the point of consumption.

  
The present invention relates to a rigid composite body or mass containing a molecular sieve based on crystalline zeolite and, optionally, a binder, said body being particularly suitable for carbonating carbonated beverages at the point of consumption if required. separate the molecular sieve from the soft drink. The rigid composite body according to the invention has a series of substantially parallel elongate channels which start from one face of said body towards the inside thereof and preferably reach its opposite face and which extend substantially along the height of the body. composite. Composite rigid bodies of the type of those of the invention provide an economical and suitable gasification system for single or multiple service of carbonated beverages.

   They can easily be combined with a container containing a suitable liquid so as to obtain an original device for the on-site carbonation of carbonated drinks.

  
An embodiment of the invention will now be described, purely by way of example, with reference to the accompanying drawings, in which:
Fig. 1 shows in perspective a composite and rigid body of crystalline zeolite according to a preferred embodiment of the invention, in the form of a thick disc traversed along its height by numerous elongated channels, substantially parallel to each other; Fig. 2 is a vertical sectional view, along the line <EMI ID = 22.1>

  
of canals, and shows in detail the structure of the composite body

  
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and containing a composite mass as shown in Figure 1; <EMI ID = 27.1> of the invention and shows the composite body shown in Figure 1 fixed inside the cover which can be fixed on a

  
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tact with the composite body by inverting the container, and Fig. 5 is a perspective view, with cutaway, of a variant of the invention, according to which the composite body shown in figure 1 is combined with a container specially designed for drinking and with the dry beverage extract for forcing. EMI ID = 29.1>

  
nomic aromatic and tasty soft drinks.

  
The description which will be given of preferred embodiments illustrated by the drawings is in no way limiting and any variant falling within the scope defined by the above claims may be adopted.

  
To obtain the carbon dioxide adsorption power necessary for the preparation of a carbonated drink at the point of

  
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and silica gel, do not have the adsorbing power necessary to

  
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sometimes also called "crystalline zeolites", can be of natural or synthetic origin. Naturally occurring aluminosilicates having molecular sieve activity include,

  
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lolite, ferrierite, chabazite, gmelinite, levynite, erionite and mordenite.

  
Since the natural crystalline aluminosilicates

  
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the methods of obtaining synthetic equivalents. There are three main types of molecular sieves based on crystalline inosilicates, which can be obtained very easily in large quantities.

  
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Zeolite A and processes for obtaining it are the subject of US Pat. No. 2,882,243. This patent gives, for the zeolite the following composition, in molar ratios of oxides:

  
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ammonium, metals of groups I and II of the periodic table and transition nets of the periodical classification

  
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up to approximately 6, the X-ray powder diffraction spectrum (or diffraction pattern) being essentially the following

  

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be replaced by conventional ion exchange methods. The sodium form of zeolite A, also called sodium zeolite A or simply NaA molecular sieve, is the easiest form of zeolite A to make. Therefore, other forms of zeolite A are generally prepared by modification of sodium zeolite A.

  
Zeolite X and processes for obtaining it are the subject of US Pat. No. 2,882,244. This patent indicates, for zeolite X, the following composition, in molar oxide ratios:

  
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not

  
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be substituted by conventional ion exchange methods. It is in the form of sodium X zeolite, also called NaX molecular sieve, that zeolite X is the easiest to manufacture and therefore the other forms of zeolite X are usually prepared by modification of sodium zeolite X.

  
Zeolite Y and a process for obtaining it are the subject of

  
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following, in molar ratios of oxides:

  
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X-rays by a powder being substantially that indicated in Table A of US Patent 3,130,007.

  
Several particular types of molecular sieves are particularly useful in the composite body useful for beverage carbonation :; according to the present invention. (The "types" of molecular sieves cited in the remainder of the description are all currently commercially available and sold by

  
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The type "4A" (NaA) has a pore size of 4 A and can

  
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o

  
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(NaX), having about 70% of its sodium cations replaced by calcium cations, is sold by Union Carbide Corp. under the name-

  
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8 A. Another molecular sieve, "Type 3A", has a structure

  
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of 3 A.

  
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crystalline aluminosilicates of the "acid resistant" category. Acid resistant molecular sieves are crystalline zeolites that do not undergo structural degradation or metal ion leaching upon prolonged contact with low pH solutions. They are usually prepared by removing

  
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exchangeable present in natural and synthetic molecular tards. To this end, ammonium ions are first substituted

  
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or replace to some extent the exchangeable metal ions of all crystalline metal aluminosilicates, complete ion exchange of this type in most cases destroys the crystal structure of the zeolite. In order to replace more "the

  
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crystalline alumina silicate, one submits to the exchanges

  
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clay-based) the latter two having a pore size of

  
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real and synthetic allowing the implementation of the inventioh with excellent results.

  
For the purposes of the invention, the substance adsorbed in the composite body of molecular sieves is of course carbon dioxide or carbon dioxide gas. Carbon dioxide is strongly adsorbed on these screens, but is easily displaced by the stronger and more preferential adsorption of water. Thus, the release, within an aqueous solution, of carbon dioxide adsorbed on molecular sieves, is the basis of the gasification process used according to the invention.

  
The total amount of carbon dioxide that can be adsorbed by molecular sieves and the rate of desorption, i.e. release by molecular sieves of carbon dioxide displaced by water molecules, vary with the size of the pores of molecular sieves. Thus, by varying the size of the pores exhibited by the molecular sieves used

  
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Different types in the formulation of the composite body affect both the rate of gasification and the final rate of gasification of the aqueous beverage.

  
Generally speaking, molecular sieves with small pores (3 to 5 and, noted, 3 to 4 A) provide

  
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relatively low. Those with larger pores (more than 6 A) ensure a release of carbon dioxide, the initial speed of which is relatively high, but which does not last very long. An aqueous solution is all the less able to dissolve carbon dioxide as it is more saturated. The dissolution of carbon dioxide

  
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excellent gasification when used according to the invention. However, the implementation according to the invention of other no-

  
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obtained with the help of such sieves excellent carbonated drinks. In general, molecular sieves should be used.

  
o

  
larvae having pores 3 to 12 A.

  
Different types of molecular sieves can also be mixed to achieve specific gasification characteristics. In cases where both a high initial release of carbon dioxide and a prolonged dissolution of this gas are desired, sieves having various pore sizes can be mixed.

  
Various shapes of molecular sieve ranging from powder

  
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are commercially available, most non-pulverulent screens comprising an inert clay-based binder at a rate of

  
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pellets (or "pellets"), formed by extrusion from 1.60 to 3.2

  
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2.38 x 1.68 ion, that is to say spheres which, for example, pass

  
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ment, these known aggregates are not very suitable for gasification

  
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to obtain, according to the invention, the mechanical strength required

  
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However, a suitable binder should normally be included in the molecular sieves. However, if the material constituting the molecular sieve has sufficient cohesion, it is unnecessary to add to it

  
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most common of these molecular sieves of coherent zeolites are synthetinucs mordenites known by the name com-

  
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that of walls of weak and appreciably uniform thickness. Any binder used should give the composite body as-

  
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the mechanical resistance provided by a suitable binder, the monolithic structures do not break into small pieces under the effect of mechanical shocks (resistance to crushing) and the molecular sieves do not come off in the form of dust during friction between the composite bodies and ur. solid neighbor (resistance to attrition).

  
Finally, the binder must be such that the mechanical resistance

  
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immerse these bodies in an aqueous drink. It is therefore necessary to use a binder capable of maintaining the mechanical strength of the composite masses in an aqueous medium, in particular at a relatively low pH, as is currently the case for carbonated drinks.

  
For the implementation of the invention, it should not be forgotten that one of the determining characteristics of composite bodies is their ability to adsorb and retain relatively large quantities of carbon dioxide in order to release them subsequently.

  
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if not determining, that the binder used according to the invention does not appreciably affect the adsorbing power of molecular sieves. Any binder exerting on the molecular sieves an action such as to reduce their adsorption capacity to below about 5% by weight relative to the unfilled mass, is not suitable for the purposes of the present invention.

  
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influence on the adsorption capacity of various molecular sieves and an effect on the rate of gas release

  
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the amount of binder incorporated into the composite body. Thus, by acting on the binder, for example by varying the type of

  
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of molecular sieve, very diverse gasification rates. Conversely, a given gasification rate can be obtained not from a single combination or unchanging proportions of binders, but from binders of various kinds or combined with molecular sieves of various types.

  
According to the invention, provision is made to bring the composite bodies of molecular sieves into intimate contact, by immersion or otherwise, with the carbonated beverage. Therefore, it is critical that the chosen binder does not introduce in the liquid beverage any inedible foreign bodies or compounds.

  
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te for not imparting an unwanted taste or aroma to the carbonating drink; however, the only essential point is that the binder does not introduce inedible or harmful substances into the aqueous beverage.

  
For the practical implementation of the invention, the binders most commonly used are mineral clays; however, it is also possible to advantageously use non-clayey binders, provided that they satisfy the aforementioned conditions, that is to say that they confer mechanical resistance to molecular sieves without affecting their adsorption capacity and not introducing any substance. or foreign compounds in the carbonating drink. Among the non-clayey binders suitable for the implementation of the invention are, for example, hydraulic or plastic cements, silicone rubber compositions and plastic resins. The examples given below illustrate the implementation according to the invention of both clayey and non-clayey binders.

  
Of course, as noted above, the most commonly used binders are clay minerals. As examples of clays capable of binding molecular sieves, mention may be made of attapulgite and clays of the attapulgite type, kaolin and clays of the kaolin type, kaolinite, sepiolite, polygars-

  
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of the bentonite type, montmorillonite, illite and chlorite. It has been determined that a combination of kaolin and bentonite based clays forms a particularly satisfactory binder which provides the composite body with mechanical strength without affecting the adsorption capacity of molecular sieves.

  
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obtained good results with clay contents not exceeding

  
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the upper limit of the content being defined only by practical possibilities. Of course, if the molecular sieves used have enough cohesion, it is unnecessary to add a binder. To form composite bodies, it is necessary to increase all the more

  
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increases relative to that of the molecular sieve, since this

  
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composite. As a result, composite bodies contain

  
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when a binder is required, suitable proportions are

  
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About 35% binder.

  
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since these do not affect the ability of bodies to carbonate aqueous drinks. By way of illustrative example, various types of optional constituents which can be incorporated into the composite bodies without affecting their gasification capacity will be cited below. Various materials, such as Texas talc or calcined talc, can be added to reduce the shrinkage experienced by the composite body during firing. Other additives can easily

  
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sodium metaphosphate, sodium tetra-pyrophosphate, or co-plasticizing agents, such as guar gum. As is well known to those skilled in the art, there are a large number of such optional constituents which can be added to composite bodies.

  
without affecting their adsorption capacity.

  
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describes several methods of making molecular sieve agglomerates. According to the teachings of the present description, those skilled in the art will be able to adapt the methods described in the US patent cited above with a view to obtaining composite bodies for the carbonation of beverages. A preferred method is to mix together the molecular sieves, a clay binder and the optional components selected by incorporating into the mixture enough moisture to be workable. The mixture is extruded through a die to obtain a long cylindrical body traversed longitudinally by elongated channels, then cut into bodies or pieces of suitable thickness which are dried and baked to activate the molecular sieves.

   The composite masses can also be closed by any other method known to those skilled in the art, for example by compression, die-casting or the like, since the method of shaping the composite bodies is not decisive in the implementation of invention.

  
During the shaping of the composite bodies of the invention, it may be necessary to remove some loose surface particles before immersing the masses in an aqueous beverage to be carbonated. This can suitably be done, before activation, by washing with water, surface grinding or other known method, in order to obtain a smooth surface which is better resistant to attrition.

  
It has been found that a monolithic gasification device

  
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cation. It has two main drawbacks, namely, the release of carbon dioxide is too slow, and it has a

  
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aqueous. This tendency is thought to result from internal pressures generated by the carbon dioxide which emerges from the molten screens.

  
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To solve these problems, it turns out to be necessary to provide a specific critical surfit, area ratio &#65533; the

  
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at the point of consumption. With this minimum specific surface

  
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release of carbon dioxide at a rate avoiding the occurrence

  
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Preferably, the specific surface of the gasification bodies

  
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Of course, the theoretical maximum specific surface area is that of an individual molecular sieve crystal. However, for the purposes of the invention, the maximum specific surface area which can practically be obtained depends only on the ability of one skilled in the art to provide a composite body having sufficient mechanical strength to withstand the shocks normally experienced during processing and handling. Practically, the maximum specific surface is about 200 cm 2 / g. Normally, the specific surface is about 6 to 50 cm2 / g and, preferably, about

  
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In carrying out the invention, it has been found that the most practical procedure for obtaining this minimum specific surface area, while keeping the composite body sufficiently

  
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The treatment and treatment is to form a composite body having a series of elongated channels which extend from one face of the body to the interior thereof and preferably reach the opposite face. According to a preferred embodiment, the composite bodies are in the form of discs, the elongate channels of which connect the two flat surfaces; however, this preferred embodiment is in no way limiting. In fact, the invention

  
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metric and of any dimensions, having channels, vacancies, alveoli, holes or cavities of any size and cross section - it is clear that those skilled in the art will be able to fabricate composite molecular sieve bodies

  
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any geometric firm, provided that it has a specific surface area within the aforementioned range. According to a variant

  
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channels and their wall thickness, which is preferably

  
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According to the invention, the composite bodies must have sufficient carbon dioxide adsorption capacity to adsorb a sufficient amount of carbon dioxide which can be released.

  
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individual posite should not only have a minimum specific surface area mentioned above, but also have a molecular sieve content, before adsorption, of about 0.17 to 1.4 ') and preferably of about 0.23 to 0.71 g per centiliter of carbonated drink. Thus, a single composite body should contain at least 6g and preferably at least 8g of molecular sieves in order to be able to adsorb enough carbon dioxide to carbonate about 34cl of aqueous beverage. Of course, if several composite bodies are to be associated with a single serving of drink or a single body

  
at a smaller portion, the amount of molecular sieve incorporated into each body should be reduced accordingly. Reciprocally, if one has to gasify a larger quantity of wood-

  
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tion.

  
The invention will now be described with reference to the des-

  
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rigid posite according to a preferred embodiment of the invention,

  
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from each other by walls 12, which in fact define the shape of the composite body. The walls? 12 define the perimeter

  
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opposite sides of the composite body to divide the interior

  
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te, as shown by way of example, because regular and favorable currents then tend to be established when placing the charged composite body in an aqueous medium. As he

  
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the channels pass right through the composite body, the gas bubbles, as they ascend, cause liquid to penetrate from below into the channels, which establishes, in a container of conventional shape, a circulation by radial symmetrical convection; this allows a greater gasification rate and the dissolution of any added flavoring and flavoring agents.

  
Figure 2 also illustrates the preferred aspect in which the channels 11 are substantially parallel to the vertical of the composite body. This orientation also contributes to the efficiency of the gasification, as the small bubbles of carbon dioxide released in each channel rise separately to the surface. If the channels extended roughly transversely to the vertical of the composite body, the carbon dioxide bubbles would almost all rise from the periphery of said body and therefore gasification would be less efficient. In the present specification, the terms "vertical" or "height" are used according to their usual meaning to denote the height of the composite body when said body is in its most stable position of equilibrium with respect to the bottom of the container in which he is placed. Good <EMI ID = 145.1>

  
that or tetrahedral, there is more than one more stable equilibrium position. In this case, the channels extend in the vertical direction of the mass occupying any of these positions.

  
By way of example of application of the invention, FIG. 3 represents the. composite body 10 according to the preferred embodiment shown in FIG. 1 disposed at the bottom of a drinking container, hereinafter denoted cup 20. The composite body can be immobilized at the base of this container using a agent

  
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10 molecular sieve monolith, charged with carbon dioxide. The container is then inverted so that the aqueous beverage comes into contact with said composite body 10, which carbonates it. After suitable carbonation of the drink, the container is turned over again so that it can be uncapped without spilling the drink. The soft drink can then be poured into glasses or beakers for individual consumption.

  
Figure 5 shows the gasification device 10 <EMI ID = 153.1>

  
gne by general reference 23, designed to serve one portion

  
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going from step 27 to a third wall section 2S ', dodeca-

  
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and console a drink.

  
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me dodecagonal chosen by way of example for the lower wall section 29 is not functionally essential for the device or assembly 23, but promotes the establishment of

  
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be sucked from top to bottom in the interstices formed between the wall section 29 and the disc 10, to circulate under and between the cells or channels (illustrated in FIG. 1) of the disc 10 to establish currents by symmetrical radial convection at the

  
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tensioned, an equivalent result would be obtained with a disc 10 with a non-circular rim, but polygonal, forming part of a circular lower wall section 29.

  
The cup 24 can be given the desired shape so that it can be fitted with similar cups in a conventional manner.

  
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bution of devices 23 because these, nested in series, are less bulky and easier to pack than an equal number

  
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Nested devices 23 can be conveniently and economically packaged in a cylindrical case, as disclosed in US Patent 3,498,798.

  
To activate the molecular sieve bodies, they are cooked at high temperatures. The minimum cooking temperature for these

  
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duit bound and remove water of hydration from molecular sieves The maximum cooking temperature is; the highest temperature

  
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optimal cooking may vary a bit depending on the combination of

  
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gasification masses. However, those skilled in the art will determine

  
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cular &#65533; or the lipnt.

  
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About 650 [deg.] C, bodies suitable for gasification according to the invention are obtained.

  
The composite bodies according to the invention are charged with carbon dioxide by simple contact of said activated bodies: with carbon dioxide under anhydrous conditions, in order to achieve the adsorption of the latter. Generally, molecular sieves can be dehydrated to a water content of about 2% by weight. It is not necessary to put the composite bodies in contact with carbon dioxide for a very long time to

  
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culars, because it is found that after only 5 minutes of such contact, the molecular sieves have adsorbed carbon dioxide at a rate of 70% of their total absorption capacity. For the purposes of the present invention, that is to say to be implemented in devices for carbonating beverages, the taris

  
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blacks 5 / * by weight (i.e. weight of adsorbed carbon dioxide / weight of molecular sieve x 100%). The de-

  
 <EMI ID = 175.1>

  
carbon dioxide at a temperature or under any pressure given either by experience or according to the degrees of edsorp-

  
 <EMI ID = 176.1>

  
Once charged with carbon dioxide, it is important that molecular sieves are packaged and stored in such a way as to avoid

  
 <EMI ID = 177.1>

  
used followed the invention. Such contact would displace the gas

  
 <EMI ID = 178.1>

  
drinks.

  
 <EMI ID = 179.1> <EMI ID = 180.1>

  
the consumer's mouth, the carbon dioxide produced the sensation

  
 <EMI ID = 181.1>

  
 <EMI ID = 182.1>

  
dissolved carbon dioxide. Gasification is generally expressed in

  
 <EMI ID = 183.1>

  
under the gasification pressure in a given volume of beverage. It is determined, in the examples below, by gravimetry by releasing the dissolved carbon dioxide by heating and by sending it, under a flow of nitrogen, into a forced absorbent layer of the product.

  
 <EMI ID = 184.1>

  
commercial sodium droxide. on an asbestos support.

  
The solubility of carbon dioxide in an aqueous solution

  
 <EMI ID = 185.1>

  
 <EMI ID = 186.1>

  
erasure and pressure, based on previous publications. There are therefore, for the gasification bodies according to the invention, certain limit temperatures and permissible pressures. The solubility of carbon dioxide in pure water is close to 0.5 volume of

  
 <EMI ID = 187.1>

  
about. Theoretically, there is no lower limit of time.

  
 <EMI ID = 188.1>

  
tically, the lower limit is of course the freezing point of the aqueous beverage to be carbonated. The particularly preferred carbonation temperature is that where the beverage is

  
 <EMI ID = 189.1>

  
 <EMI ID = 190.1> <EMI ID = 191.1>

  
to that generally carried out using types of molecular sieves and clay binders other than those mentioned in the examples given below.

  
The nature of the carbonated drink according to the invention is not critical. This drink must of course be aqueous. It may contain, in addition to water, any flavoring and flavorful agent, a coloring agent, a food additive, a drug or an alcohol, these agents having no detrimental action. We can,;

  
 <EMI ID = 192.1>

  
milks loaded with carbon dioxide, which can then be used to prepare, from tap water, flavored and tasty carbonated drinks. According to another variant of the invention, an aqueous mixture of aromatic and tasty agency can be provided. and dyes, which are added to the water in which it is immersed so-

  
 <EMI ID = 193.1>

  
fuck. As examples of the type: - of drinks which can be prepared from suitable liquids by gasification according to the invention.

  
 <EMI ID = 194.1>

  
nales, beer and sparkling wine.

  
However, certain solutes possibly present in aqueous beverages which may affect the dissolution of carbon dioxide and certain preferred embodiments of

  
 <EMI ID = 195.1> <EMI ID = 196.1>

  
limit this type of gasification. For example, fructose,

  
 <EMI ID = 197.1>

  
 <EMI ID = 198.1>

  
holding. However, it has been found that molecular tarais having

  
0

  
 <EMI ID = 199.1>

  
 <EMI ID = 200.1>

  
 <EMI ID = 201.1>

  
 <EMI ID = 202.1>

  
 <EMI ID = 203.1>

  
sounds by molecular sieve bodies. However, these drinks containing such acids necessarily have a fairly low pH;

  
 <EMI ID = 204.1>

  
is 2). Prolonged contact of such solutions with many

  
 <EMI ID = 205.1>

  
gradual viation of metal ions from the sieve. This may result in an increase in pH sufficient to significantly affect

  
 <EMI ID = 206.1>

  
according to the invention aqueous drinks containing edible acids, it is preferable to use molecular sieves

  
 <EMI ID = 207.1>

  
solution from molecular sieves does not dissolve as well as when the release is slower. In general, a slower release offers more facilities for gas-liquid contact and therefore promotes the dissolution of carbon dioxide. As previously indicated, a method of slowing down the movement

  
 <EMI ID = 208.1>

  
laries consists of using molecular sieves, some of which

  
o

  
 <EMI ID = 209.1>

  
 <EMI ID = 210.1>

  
of dissolution 'of carbon dioxide in a solution is an inverse function of the degree of saturation thereof. This relationship mows

  
 <EMI ID = 211.1> <EMI ID = 212.1>

  
aqueous beverage Further, while in a carbonated beverage the absolute degree of carbonation is important for the beverage to satisfy the consumer, it has been found that the "apparent" degree of carbonation, i.e., the release in the drink of small bubbles of carbon dioxide, shows an apparent gasification. Consequently, in the industrial use of composite bodies according to the invention as gasification discs

  
 <EMI ID = 213.1>

  
molecules at a rate greater than that at which it can go into solution, so that it can be seen to bubble out of solution.

  
For certain applications, it may be advisable to use, in combination, molecular sieves and a chemical couple. ) In general, the cost price of chemical couples,

  
 <EMI ID = 214.1>

  
that of molecular sieves. The foreign taste communicated by salts formed by carbon dioxide from chemical couples is zero or barely perceptible for a low dose of salts

  
'(it varies with the nature of the constituents of the chemical couple,

  
that of the aromatic and tasty agents present in the drink and the acuity of the consumer). Generally, a weak gasification (0.5 to 0.75 volume of dissolved carbon dioxide) in a cola-based gas can be achieved by using a chemical couple without excessive formation of salts introducing a foreign taste. Accordingly, it is advantageous to ensure a low degree of gasification with the aid of a chemical couple and to supplement the gasification with the aid of molecular sieves. In view of '

  
This mixed effect, it may be advantageous to use molecular sieves having small pores (about 3 to 5 A) to cause a slow release which complements the rapid release provided by the chemical couple. When this mixed method is adopted, the composite bodies with multiple elongated channels make it possible to conveniently separate the acid and basic constituents of the chemical couple. Elongated channels provide a clean receptacle

  
keeping the two components separate until the composite body is immersed in the aqueous beverage. It is only at the moment

  
where the two constituents dissolve as the chemical couple

  
 <EMI ID = 215.1> <EMI ID = 216.1>

  
during the immersion of said body in the drink.

  
The invention will be described in more detail by means of the illustrative examples below given without limitation.

EXAMPLE I-

  
Rigid composite bodies of molecular sieves were prepared according to the following procedure; we mixed during. approximately 4 minutes, in a planetary bladed mixer of the "Hobart" Model C-100 "type, rotating at 60 rpm, 726 g of sodium Y zeolite having a moisture content * of 41.74% (such as that

  
 <EMI ID = 217.1>

  
100 g of a clay binder formed from a mixture of approximately 50% of

  
 <EMI ID = 218.1>

  
of Texas, Texas talc, calcined talc and feldspar (this mixture being sold by Georgia Kaolin Company under the trade name of "Prepared Wall Tile Body"). Then 15 g of sodium silicate solution was added to the mixture and mixing continued for a further 4 minutes. Without stopping the m-

  
 <EMI ID = 219.1>

  
1 minute, then kneading was continued for another 10 minutes, to form the mixture into a plastic mass

  
 <EMI ID = 220.1>

  
"Enerpac", the plastic mass was extruded through a single die to form a cylinder-shaped extrudate containing small longitudinal and square-section channels separated by thin walls. This cylinder was cut into disks using a thin wire. The disks had approximately the following dimensions:

  

 <EMI ID = 221.1>


  
 <EMI ID = 222.1>

  
The molecular sieve discs were then removed.

  
on a wire rack and dried in a draft for about 16 hours at room temperature (about
21 [deg.] C). The dried disks were placed in a baking oven

  
 <EMI ID = 223.1>

  
t \ <EMI ID = 224.1>

  
ment the temperature up to 600 [deg.] C in about an hour. The molecular sieves were kept at 600 [deg.] C for 5 hours to cook them.

  
 <EMI ID = 225.1>

  
unit was about 15g.

  
The heated discs were removed from the oven and passed directly into a metal container having a tightly closing lid and inlet and outlet holes allowing gas to pass through it. We took us through the reci-

  
 <EMI ID = 226.1>

  
atmospheric pressure, and the discs have adsorbed some of this gas. The total carbon dioxide adsorbed at the end of this loading time was 2.63 g.

  
We removed the discs, then brought back to a warming temperature, from the metal container and placed them in glass bottles, which were capped. immediately to protect discs from

  
 <EMI ID = 227.1>

  
proud a watery drink.

  
A disc prepared and charged with carbon dioxide was placed according to the procedure described above in an empty cup.

  
 <EMI ID = 228.1>

  
of commercially available cola, then filled the cup with water. There was a rapid release of carbon dioxide in the form of many small gas bubbles and one obtained in monks .. of a minute a sparkling and effer-

  
 <EMI ID = 229.1>

  
nique, common carbonated drinks, and exhibited no foreign flavor or aroma. The evolution of gas bubbles continued for more than 8 minutes. Subsequent examination revealed that neither the shape nor the dimensions of the disc were altered.

  
 <EMI ID = 230.1>

  
 <EMI ID = 231.1>

  
at the base of the cup so that it is an integral part of the latter. A cola drink was then prepared as described above.

  
 <EMI ID = 232.1>

  
 <EMI ID = 233.1>

  
it <EMI ID = 234.1>

  
another disc, similar to the previous ones, we obtained the following results:

  

 <EMI ID = 235.1>

EXAMPLE II

  
A homogeneous, wet plastic mixture was prepared for extrusion using the same materials, compositions, instruments and procedures as in Example I. The mixture was divided.

  
 <EMI ID = 236.1>

  
Fraction A was extruded according to the procedure

  
 <EMI ID = 237.1>

  
of a flat die. The resulting profile was cut into discs, each of which had 120 channels as before. Fraction B was subjected to a similar extrusion, but with the die removed from the extruder. The resulting extrudate was a solid cylinder 50.8 mm in diameter, cut with wire into solid discs of the same thickness or height as the discs obtained from fraction A. Of course, the discs formed from fraction B did not have the longitudinal channels connecting the opposite faces of the discs obtained from fraction A.

  
The discs formed from fractions A and B were dried, heated and loaded with equal amounts.

  
 <EMI ID = 238.1>

  
Subsequent analyzes showed that the rate of drying

  
 <EMI ID = 239.1> <EMI ID = 240.1>

  
 <EMI ID = 241.1>

  

 <EMI ID = 242.1>


  
Disc B did not produce gas evolution fast enough to properly carbonate a beverage, while disc A did provide high quality carbonated drinks. EXAMPLE III-

  
Example II was repeated by subjecting to the extrusion a medium.

  
 <EMI ID = 243.1>

  
of bentonite and corresponding increase in the percentage of Texas figulin clay, Texas talcum and feldspar, so that the final weight of the mixture was the same.

  
As in Example II, two sets of discs were prepared, those of set A each having 120 channels and those of set B being solid or solid, that is to say free.

  
of channels. All the disks were dried, heated and charged with carbon dioxide as in Example II. Analyzes showed that the gasification rate was much greater for A disks than for B disks, the average degrees

  
 <EMI ID = 244.1>

  

 <EMI ID = 245.1>


  
The gas evolution produced by the discs B was too slow to ensure good gasification. The A discs produced high quality carbonated drinks upon immersion in aqueous solutions.

EXAMPLE IV-

  
Four different mixtures were prepared for extrusion using the same equipment and according to the procedure described in Example I. These mixtures A, B, C and D had (in g) the following compositions:

  

 <EMI ID = 246.1>


  
 <EMI ID = 247.1>

  
 <EMI ID = 248.1>

  
canals. This extrudate was cut into discs each having
80 channels, which we have dried, heated and loaded with carbon dioxide as in example J, except that we operated on

  
 <EMI ID = 249.1>

  
24 hour time.

  
Analyzes have shown that the proportion of binder affects

  
 <EMI ID = 250.1>

  
for A discs, medium speed for B and C discs

  
and slow for D disks. However, all compositions have given disks suitable for the practice of the invention. EXAMPLE V-

  
Example IV was repeated using the same material and

  
 <EMI ID = 251.1>

  
 <EMI ID = 252.1>

  
trusion three mixtures having (in g) the following compositions:

  

 <EMI ID = 253.1>


  
Analyzes made on the loaded disks showed that the gasification rate was extremely high for the A disks, intermediate for the B disks and low for the C disks. All the compositions gave the disks.

  
 <EMI ID = 254.1> <EMI ID = 255.1>

EXEMPTED VI-

  
 <EMI ID = 256.1>

  
The mixture subjected to the extrusion had the following composition:

  

 <EMI ID = 257.1>


  
The discs were dried for 6 minutes in a microwave oven of 11 kW power. The discs were then heated for 6 hours at 600 [deg.] C, as in Example I. After heating ,we have. stored the discs in closed bottles

  
 <EMI ID = 258.1>

  
 <EMI ID = 259.1>

  
under a nitrogen atmosphere. The discs were then exposed, for various times, to an atmosphere of anhydrous carbon dioxide. Immediately after this exposure, the discs were reweighed under an atmosphere of dry nitrogen. The quantity of carbon dioxide adsorbed by each disc was then calculated according to the following equation:

  

 <EMI ID = 260.1>


  
where A is the percentage of adsorbed carbon dioxide, I the initial weight (before loading) of the disc in grams and F the final weight

  
 <EMI ID = 261.1>

  
following results:

  

 <EMI ID = 262.1>
 

  
 <EMI ID = 263.1>

  
to effectively carbonate a carbonated drink in which it has been placed.

EXAMPLE VII

  
A number of molecular sieve discs were extruded using the same materials and compositions, equipment and methods as in Example I.

  
 <EMI ID = 264.1>

  
 <EMI ID = 265.1>

  
dried in four groups, which were subjected to baking at different temperatures for 6 hours. All the discs were then charged with carbon dioxide for 16 hours under a

  
 <EMI ID = 266.1>

  
weight average carbon dioxide adsorbed by three disks in each group, weighing, as described in Example VI, the disks before and after loading. The results are as follows:

  

 <EMI ID = 267.1>


  
The ability of the D-discs to adsorb gas was completely destroyed by the high firing temperature. Examination of the immersed discs, after the end of gas evolution,

  
showed that the discs: had less mechanical strength than the others, but were still acceptable for use according to the invention.

  
 <EMI ID = 268.1>

  
 <EMI ID = 269.1>

  
culars according to the invention mixed for about 3

  
 <EMI ID = 270.1> <EMI ID = 271.1>

  
suitable for forming the composite bodies * according to the invention.

  
Based on the initial moisture contents of the dry constituents

  
 <EMI ID = 272.1>

  
a moisture content of 42.9%.

  
 <EMI ID = 273.1>

  
 <EMI ID = 274.1>

  
cylindrical, contained 80 small longitudinal channels, parallel to each other, with a square section, separated by thin walls. We

  
 <EMI ID = 275.1>

  
gasification having 80 channels going from one flat face to the other.

  
After air drying for about 16 hours to about
20 [deg.] C, the discs were baked for 6 hours at 600 [deg.] C, then charged with carbon dioxide for 6 hours, under atmospheric pressure.

  
The gasification properties of various discs were then determined and all were found to be substantially equal. The average results obtained are as follows:

  

 <EMI ID = 276.1>


  
Another record was placed in an empty one-container cup.

  
 <EMI ID = 277.1>

  
very commercially available and the cup was filled with water. A rapid evolution of gas bubbles occurred and a sparkling and effervescent carbonated drink was obtained. On tasting the carbonated cola drink, no foreign flavor or aroma was detected and examination revealed that the disc had not undergone any change in shape or size. EXAMPLE IX-

  
 <EMI ID = 278.1>

  
milks according to the invention by mixing intimately for about

  
 <EMI ID = 279.1>

  
1 1) <EMI ID = 280.1>

  
 <EMI ID = 281.1>

  
cooked for 6 hours at 800 [deg.] C under atmospheric pressure. Cn

  
 <EMI ID = 282.1>

  
 <EMI ID = 283.1>

  
 <EMI ID = 284.1>

  
of commercially available cola and water, there was obtained a sparkling carbonated drink without any foreign flavor or flavor and containing no particles detached from the carbonating disc. EXAMPLE

  
Rigid composite bodies of molecular sieves according to the invention were prepared by mixing: 43.5 parts of powder of

  
 <EMI ID = 285.1>

  
 <EMI ID = 286.1>

  
silicone rubber foam base. After kneading the mixture well, the silicone rubber binder catalyst was added thereto and stirred quickly and vigorously to

  
form a homogeneous mass which was then placed in a cylindrical mold. Channels were then made in the flat faces of the cy-

  
 <EMI ID = 287.1>

  
series of studs. After a few minutes, the mixture is

  
 <EMI ID = 288.1>

  
discs approximately 13 mm thick. We heated the records to
300 [deg.] C for four hours to dehydrate them and activate molecular sieves. Cn then exposed the discs to gas

  
 <EMI ID = 289.1>

  
for the adsorption of CO2.

  
 <EMI ID = 290.1>

  
 <EMI ID = 291.1>

  
 <EMI ID = 292.1>

  
trade, sweetened to the desired dose for the drink, and the cup was filled with water. Gas evolution has occurred

  
 <EMI ID = 293.1>

  
cola-based soft drinks in bottles had conferred.

  
 <EMI ID = 294.1>

  
carbon dioxide, carbonated drinks, and was free of this flavor

  
 <EMI ID = 295.1>

  
 <EMI ID = 296.1>

  
long effervescent.

  
Substantially the same results were obtained by adding the

  
 <EMI ID = 297.1>

  
 <EMI ID = 298.1>

  
 <EMI ID = 299.1>

  
silicone rubber foam had resistance to

  
 <EMI ID = 300.1>

  
 <EMI ID = 301.1>

  
knife all these discs without noticing the presence of powder detached as a result of the cutting.

  
Thus, it can be seen that, according to the invention, a rigid composite body has been obtained, containing crystalline molecular sieves and internally exhibiting channels permeable to liquids, which enables the objects of the present invention to be fully achieved. Of course, it will be possible to provide the modes of implementation of. written by way of example all modifications and variations obvious to horror: ne of the art without departing from the scope of the invention, defined by the claims below.

  
 <EMI ID = 302.1>

  
 <EMI ID = 303.1>

  
of said body.

  
 <EMI ID = 304.1>


    

Claims (1)

<EMI ID = 305.1> has adsorbed a releasable quantity of carbon dioxide sufficient to <EMI ID = 306.1> his. 3. Body according to claim 1, characterized in that it <EMI ID = 307.1> crystalline distributed practically uniformly within said body. 4. Rigid composite body according to claim 1 useful for the individual carbonation of portions of aqueous drinks. <EMI ID = 308.1> molecules based on crystalline zeolite, said body having <EMI ID = 309.1> <EMI ID = 310.1> <EMI ID = 311.1> of carbon dioxide sufficient to carbonate an aqueous beverage when immersed in said carbonate beverage. <EMI ID = 312.1> that it contains about 0.23 to 0.71 g of uncharged molecular sieves per centiliter of aqueous carbonated beverage. 6. Rigid composite body, characterized in that it <EMI ID = 313.1> lite crystalline, in that it has a series of substantially parallel elongate channels extending from one of its faces to its opposite face, practically along the vertical of said body, said body <EMI ID = 314.1> a quantity of carbon dioxide sufficient to carbonate, releasing this gas, an aqueous drink when it is immersed in said drink. <EMI ID = 315.1> <EMI ID = 316.1> <EMI ID = 317.1> <EMI ID = 318.1> 9. Body according to claim 8, characterized in that it <EMI ID = 319.1> <EMI ID = 320.1> 11. Body according to any one of claims 1 to 10, characterized in that it has a specific surface area of approximately 6 to 50 c: n2 / g. 12. Body according to any one of claims 1 to 11, characterized in that it has a specific surface area of approximately <EMI ID = 321.1> <EMI ID = 322.1> in that it has a series of substantially parallel elongated channels which extend from one face of said body inwardly of said body, the longitudinal axis of said channels being substantially parallel to the vertical axis of said body. 14. Body according to claim 13, characterized in that said elongated channels extend from one desaites faces of said body to the opposite face. 15. Device for the carbonation of a drink, characterized in that it comprises a composite rigid body containing at least 40% by weight of molecular sieves based on crystalline zeolite, in that it has a series of substantially elongated channels. parallel which extend from one of its faces to its opposite face, the longitudinal axis of said channels being substantially parallel to the vertical axis of said body, said body having a <EMI ID = 323.1> <EMI ID = 324.1> <EMI ID = 325.1> <EMI ID = 326.1> suitable for containing liquids. 16. Device according to claim 15, characterized in that said composite body is as defiai in one <EMI ID = 327.1> <EMI ID = 328.1> these towards its interior, the longitudinal axis of said channels being <EMI ID = 329.1> <EMI ID = 330.1> quantity of carbon dioxide sufficient to carbonate, releasing this Gas, an aqueous drink when it is immersed in said drink and, on the other hand, a drinking vessel in which said ccrps is fixed so as to form substantially an integral part of said container when said device is used for carrying out gasification. 18. Device according to claim 17, characterized in that said composite body is as defined in any one of claims 1 to 11. 19. Device according to claim 17, characterized in that said composite body is under the force of a disc having <EMI ID = 331.1> has approximately 75 to 225 elongated channels extending from one of its flat faces to its opposite flat face, the walls which separate these channels <EMI ID = 332.1> 20. Device according to claim 17, characterized in that the drinking vessel is provided with a circular cover intended to protect said composite body from atmospheric humidity. 21.Device according to claim 20, characterized in that <EMI ID = 333.1> junction between two wall sections of this container. <EMI ID = 334.1> that the cover is removably held on said step by a series of pins directed inwards. 23. Device according to claim 17, characterized in that the drinking container is designed so that one can fit <EMI ID = 335.1>