WO2022029672A1 - Method for activation of a natural zeolite - Google Patents
Method for activation of a natural zeolite Download PDFInfo
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- WO2022029672A1 WO2022029672A1 PCT/IB2021/057188 IB2021057188W WO2022029672A1 WO 2022029672 A1 WO2022029672 A1 WO 2022029672A1 IB 2021057188 W IB2021057188 W IB 2021057188W WO 2022029672 A1 WO2022029672 A1 WO 2022029672A1
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- natural zeolite
- electric field
- time interval
- buffer solution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
Abstract
A method for activation of natural zeolite comprises the steps of subjecting natural zeolite in succession to a washing step with a mild saline solution and to an electric field with a square wave current flow for a predetermined time interval, to a first treatment with a sulphate buffer solution having a pH of 5.6 and to an electric field with a square wave current flow for a predetermined time interval, to a second treatment with a phosphate buffer solution having a pH of 6.0 and to an electric field with a square wave current flow for a predetermined time interval, to a third treatment with a phosphate buffer solution having a pH of 6.8 and to an electric field with a square wave current flow for a predetermined time interval, and to washing with a demineralized water and to an electric field with a square wave current flow for a predetermined time interval.
Description
METHOD FOR ACTIVATION OF A NATURAL ZEOLITE
TECHNICAL SECTOR
The present invention relates to the sector of processes for the treatment of aluminosilicates. The present invention has been developed with particular regard to activated natural zeolite and to a method for activation of natural zeolite.
PRIOR ART
Natural zeolite is a mineral of volcanic origin, the crystalline structure of which determines its porosity. Its name is derived from Greek and refers to its capacity to develop steam (or smoke) internally when subjected to heating. The "smoke" is derived from the particles of water retained inside its porous structure.
Natural zeolite is able to bond many substances such as, merely by way of example, heavy metals and at the same time is able to exert a strong anti-radical action due to its properties.
For this reason, natural zeolite is able to exert a beneficial action against all those compounds which, via an oxidation process, produce an alteration of the organoleptic properties of beverages and food matrices in general.
There is also another aspect which contributes substantially to the potential action exerted by natural zeolite; this mineral, in fact, is not toxic for the human body and cannot be absorbed by the gastro-intestinal tract and therefore, when it passes through it, may only perform its dual antioxidant and purifying action in respect of all those substances and compounds which, introduced with food, could alter the normal cellular physiological state leading to a condition of oxidative stress.
Natural or synthetic zeolite is used in the agricultural and food industry as an improver and/or integrator. In this respect zeolite may undoubtedly have a wide range of possible applications in view of its potential benefits fundamentally associated with its molecular structure and chemical-physical characteristics and properties derived therefrom.
Therefore the need has arisen to enhance the properties of this mineral in order to improve further the effects produced both in relation to food and in different areas of application.
Numerous experiments carried out by the Proprietor have shown how natural zeolite can, so to speak, be "activated" if subjected to a predetermined preparation method which produces a different action thereof when applied during the structuring and formulation of the end product. For example, but not exclusively, activated natural zeolite may be used to produce beverages and/or food matrices with an improved nutraceutical value.
When applied to food products, activation of the natural zeolite, in addition to having a direct action resulting from the treatment performed on the natural zeolite, heightens the intrinsic properties of the matrix, understood as being the material and/or substance to be conditioned, improving both the availability thereof in bioactive compounds present and the stability over time.
The object of the present invention is therefore to satisfy the aforementioned need by providing activated natural zeolite which is able to improve the nutraceutical characteristics of the product with which it is associated.
Another object of the present invention is to provide a method for activation of natural zeolite which is simple to implement, which is easily repeatable and which is inexpensive to realize.
These objects are achieved by the characteristic features of the invention illustrated in the independent claim 1 . The dependent claims define preferred and/or particularly advantageous aspects of the invention.
SUMMARY OF THE INVENTION
In accordance with the aforementioned objects, the present invention provides a method for activation of natural zeolite comprising the steps of subjecting natural zeolite: to washing with a mild saline solution and to an electric field with a square wave current flow for a predetermined time interval; to a treatment with a sulphate buffer solution having a pH of 5.6 and to an electric field with a square wave current flow for a predetermined time interval; to a first treatment with a phosphate buffer solution having a pH of 6.0 and to an electric field with a square wave current flow for a predetermined time interval; to a second treatment with a phosphate buffer solution having a pH of 6.8 and to an electric field with a square wave current flow for a predetermined time interval; and to washing with demineralized water and to an electric field with a square wave current flow for a predetermined time interval;
Owing to this solution it is possible to modify the polar state of the zeolite, increasing the number of positive charges available and causing a specific action thereof when it is added to a predetermined matrix.
According to another aspect of the present invention, the washing step with a mild saline solution comprises the following steps:
subjecting the natural zeolite to a forced circulation of the mild saline solution continuously for a time interval of between 5 and 10 minutes in the absence of an active electric field; interrupting the forced circulation of the mild saline solution; subjecting the natural zeolite to an electric field with a square wave current flow for a time interval of between 8 and 12 minutes; deactivating the electric field; and subjecting the natural zeolite to a forced circulation of the mild saline solution for a time interval of between 4 and 8 minutes.
Owing to this solution it is possible to remove any compounds present within the natural zeolite, such as metals and/or other cations.
According to another aspect of the present invention, the first treatment step with sulphate buffer solution comprises the steps of: subjecting the natural zeolite to a forced circulation of the buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field; interrupting the forced circulation of the buffer solution; activating an electric field with a square wave current flow for a time interval of between 3 and 7 minutes; deactivating the electric field; and subjecting the natural zeolite to a forced circulation of the buffer solution continuously for a time interval of between 1 and 5 minutes.
According to a further aspect of the present invention, the second treatment step with phosphate buffer solution comprises the steps of:
subjecting the natural zeolite to a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field; interrupting the forced circulation of the phosphate buffer solution; subjecting the natural zeolite to an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; deactivating the electric field; and subjecting the natural zeolite to a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes.
According to a further aspect of the present invention, the third treatment step with phosphate buffer solution comprises the steps of: subjecting the natural zeolite to a first forced circulation of the buffer solution continuously for a time interval of between 1 and 6 minutes in the absence of an active electric field; interrupting the first forced circulation of the phosphate buffer solution; subjecting the natural zeolite to an electric field with a square wave current flow for a time interval of between 8 and 12 minutes; deactivating the electric field; and subjecting the natural zeolite to a second forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes; interrupting the second forced circulation of the phosphate buffer solution; subjecting the natural zeolite to a third forced circulation of the phosphate buffer solution continuously for a time interval of between 4 and 8 minutes. interrupting the third forced circulation of the phosphate buffer solution;
subjecting the natural zeolite to an electric field with a square wave current flow for a time interval of between 12 and 18 minutes; deactivating the electric field.
According to a further aspect of the present invention, the washing step with demineralized water comprises the steps of: subjecting the natural zeolite to a forced circulation continuously of a first predetermined quantity of demineralized water for a time interval of between 3 and 7 minutes in the absence of an active electric field; deactivating the forced circulation and subjecting the natural zeolite to an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; and deactivating the electric field.
A further aspect of the present invention involves a step of storing the natural zeolite in an air-free environment.
Owing to this solution it is possible to keep the natural zeolite stable and activated for a long period of time, even for up to thirty-six months.
According to another aspect of the present invention, before the first step of washing the natural zeolite with mild saline solution, the method also comprises a pretreatment step, comprising the steps of: screening the natural zeolite according to the particle size, and separating the screened natural zeolite from the rest of the natural zeolite.
Owing to this solution it is possible to optimize the activation method, using natural zeolite with a particular particle size, a specific porosity and, at the same time, a well- defined physical chemical structure thereof.
According to a further aspect, the present invention involves the steps of preparing:
a container, a voltage generator, and two armatures arranged at the two ends of the tank and electrically connected to the two terminals of the voltage generator so as to form, respectively, the positive pole and the negative pole of a dipole, and placing the natural zeolite inside the container.
According to a further aspect of the present invention it is envisaged that: during the washing step with mild saline solution the natural zeolite is placed at the positive pole, during the first treatment step with a sulphate buffer solution the natural zeolite is placed at the negative pole, during the second treatment step with a phosphate buffer solution the natural zeolite is placed at the negative pole, during the third treatment step with a phosphate buffer solution the natural zeolite is placed at the negative pole, and during the washing step with demineralized water the natural zeolite is placed close to the positive pole.
BRIEF DESCRIPTION OF THE DRAWINGS
Further characteristic features and advantages of the present invention will become clear from the following description, provided solely by way of example with reference to the attached drawings in which:
Figure 1 shows a schematic view of a treatment device according to the present invention; and
Figure 2 is a graph showing the results of the analyses carried out on a beverage to which activated natural zeolite according to the present invention had been added.
In order to facilitate understanding, identical reference numbers have been used, where possible, to identify identical common elements in the figures. It is understood that elements or characteristics of one embodiment may be conveniently incorporated in other embodiments without further clarifications.
PREFERRED MODE OF IMPLEMENTATION OF THE INVENTON
Reference will now be made in detail to the various embodiments of the invention, one or more examples of which are shown in the attached figures. Each example is provided merely by way of illustration of the invention and is understood as not constituting a limitation thereof. For example, the technical characteristics shown or described since they form part of an embodiment may be integrated within, or associated with, other embodiments in order to produce a further embodiment. It is understood that the present invention will be inclusive of these modifications and variants.
It is emphasized moreover that the present description is not limited in its application to the constructional details and arrangement of the components as described below using the attached figures. The present description may envisage other embodiments and be realized or implemented in practice using other typically equivalent characteristics. The terms used below have a purely descriptive purpose and must not be regarded as being limiting.
The research and development activity conducted by the Proprietor has resulted in the development of an innovative and particular biotechnological process which allows the production of innovative intermediate products in combined form.
Reference is made to intermediate products since the activation method described provides a product which is to be added to the different types of matrices, conditioning them in turn and providing them with improved nutraceutical properties which cannot be obtained except by means of the application and addition of activated natural zeolite.
Very succinctly, it consists of a process for conditioning an active natural mineral which, if applied, is able to improve the characteristics of the matrix to be treated.
Considering the properties of the mineral, the research has shown how the use of a particular type of natural zeolite associated with a specific treatment has enabled the predefined objects to be achieved. The results obtained from the implementation of a rigorous research and testing program aimed at characterizing the method for treatment of the mineral described are the result of a repeated series of operations and analyses carried in two different phases and in triplicate. It should be pointed out that the data obtained allows the formulation of specific certification procedures depending on the different applications (different matrices treated), and therefore the application of treated, or activated, natural zeolite allows the development in cascade of further protection processes for the single products to be obtained.
The natural zeolite activation method comprises a series of steps during which the zeolite is subjected to different treatments, such as by way of example, but not exclusively, the application of a dipole with constant voltage in a predetermined buffer solution.
According to one of the embodiments of the present invention, some steps of the method are performed inside a treatment device, denoted generically in the attached figures by the number 10. During these steps, the natural zeolite 1 is subjected to the action of an electric field.
The device 10 comprises a container 20, for example a tank, and a voltage generator 30. Two armatures 32, 34 are electrically connected to the two terminals of the voltage generator 30 so as to form, respectively, the positive pole 32 and the negative pole 34 of a dipole. The armatures 32, 34 may be arranged at the two ends of the tank 20.
The dipole supplies a current flow in the form of a constant voltage square wave where the current, and consequently the applied electric field, cause a kind of pulse dispensing action with uniform alternation of two voltage values, each of which is maintained for a predetermined time interval. The highest voltage value is between 50 and 140 V. The transition times between the two voltage values, leading edge and trailing edge, are extremely short, i.e. instantaneous.
Natural zeolite 1 is preferably arranged inside one or more containers 40. According to a particularly advantageous characteristic of the present invention, the width of the containers 40 containing the natural zeolite 1 , occupies at the most a distal third of the distance between the two poles 32, 34.
The system also comprises one or more pumps connected to the tank 20 and a hydraulic circuit outside the tank 20, which together allow the forced circulation of liquids inside the tank 20. The external hydraulic circuit may be selectively emptied to allow changing of the liquid used in the forced circulation. As will become clearer below, these pumps are in fact used for the forced circulation of a saline solution, various types of buffer solutions and/or water for allowing the implementation of the method according to the present invention.
The method for activation of natural zeolite 1 comprises a first step during which the natural zeolite is subjected to washing with a mild saline solution. The term "mild saline solution" is understood as meaning in the present description a saline solution
in which the concentration of sodium chloride is between 1% and 2%, for example between 8 and 18 g/L, preferably, but not exclusively 12 g/L.
The first step of washing natural zeolite with a mild saline solution involves the insertion of a predetermined quantity of saline solution inside the tank 20 and comprises, in turn, the following steps: activating a forced circulation of the saline solution continuously for a time interval of between 5 and 10 minutes in the absence of an active electric field, namely with the voltage generator 30 switched off; interrupting the forced circulation of the mild saline solution; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 8 and 12 minutes; switching off the voltage generator 30 in order to deactivate the electric field; and activating a forced circulation of the saline solution for a time interval of between 4 and 8 minutes.
At the end of the first washing step, the method comprises a step of extraction of the mild saline solution from the tank 20.
According to a particularly advantageous characteristic feature, during this treatment step the containers 40 containing natural zeolite 1 may be placed close to or at the positive pole 32.
In the present description the terms "close to" or "at" with reference to the position of the zeolite with respect to one of the poles of the dipole is understood as meaning that the distance of the zeolite from said pole is greater than the distance of the zeolite from the opposite pole. In a configuration in which each pole, namely each armature 32, 34, is arranged at one end of the tank 20, these terms indicate that the
zeolite 1 is arranged inside the tank in a position such that the distance of the zeolite 1 from one of the ends of the tank 20 is greater than the distance of the zeolite 1 from the opposite end of the tank 20.
The method for activation of natural zeolite 1 further comprises a first step of treatment of the natural zeolite 1. During this step the natural zeolite 1 is placed in contact with a sulphate buffer solution having an acidity value of between 5 and 6 pH, preferably with a pH of 5.6.
The first step of treatment of the natural zeolite 1 with a sulphate buffer solution involves the insertion of a predetermined quantity of sulphate buffer solution with a pH of 5.6 inside the tank 20 and comprises, in turn, the following series of steps: activating a forced circulation of the sulphate buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field, namely with the voltage generator 30 switched off; interrupting the forced circulation of the sulphate buffer solution; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 3 and 7 minutes; switching off the voltage generator 30 in order to deactivate the electric field; and activating a forced circulation of the sulphate solution continuously for a time interval of between 1 and 5 minutes.
At the end of the first treatment step, the method comprises a step of extraction of the sulphate buffer solution from the tank 20.
According to a particularly advantageous characteristic feature, during this treatment step the containers 40 containing natural zeolite 1 may be placed close to or at the negative pole 34.
The method for activation of natural zeolite 1 further comprises a second step for treatment of natural zeolite 1. During this step the natural zeolite 1 is placed in contact with a phosphate buffer solution having an acidity value of between 5.5 and 6.7 pH, preferably with a pH of 6.0.
The second step for treatment of natural zeolite 1 with a phosphate buffer solution involves the insertion of a predetermined quantity of phosphate buffer solution with a pH of 6.0 inside the container 20 and comprises, in turn, the following series of steps: activating a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field, namely with the voltage generator 30 switched off; interrupting the forced circulation of the phosphate buffer solution; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; switching off the voltage generator 30 in order to deactivate the electric field; and activating a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes.
At the end of the second treatment step, the method comprises a step of extraction of the phosphate buffer solution from the tank 20.
According to a particularly advantageous characteristic feature, during this treatment step the containers 40 containing natural zeolite 1 may be placed close to or at the negative pole 34.
The method for activation of natural zeolite 1 further comprises a third step for treatment of the natural zeolite 1. During this step the natural zeolite 1 is placed in
contact with a phosphate buffer solution having an acidity value of between 6.5 and 7.5 pH, preferably with a pH of 6.8.
The third step for treatment of natural zeolite 1 with a phosphate buffer solution involves the insertion of a predetermined quantity of phosphate buffer solution with a pH of 6.8 inside the tank 20 and comprises, in turn, the following series of steps: activating a first forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 6 minutes in the absence of an active electric field, namely with the voltage generator 30 switched off; interrupting the first forced circulation of the phosphate buffer solution; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 8 and 12 minutes; switching off the voltage generator 30 in order to deactivate the electric field; and activating a second forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes. interrupting the second forced circulation of the phosphate buffer solution; activating a third forced circulation of the phosphate buffer solution continuously for a time interval of between 4 and 8 minutes. interrupting the third forced circulation of the phosphate buffer solution; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 12 and 18 minutes; switching off the voltage generator 30 in order to deactivate the electric field.
At the end of the third treatment step, the method comprises a step of extraction of the phosphate buffer solution from the tank 20.
According to a particularly advantageous characteristic feature, during this treatment step the containers 40 containing natural zeolite 1 may be placed close to or at the negative pole 34.
The activation method also comprises a second step of washing the natural zeolite 1 , during which the natural zeolite 1 is placed in contact with demineralized water.
The washing step with demineralized water involves the insertion of a predetermined quantity of demineralized water inside the tank 20 and comprises, in turn, the following series of steps: activating a forced circulation continuously of the demineralized water for a time interval of between 3 and 7 minutes in the absence of an active electric field; interrupting the forced circulation; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; switching off the voltage generator 30 in order to deactivate the electric field.
According to one of the alternative embodiments of the present invention, the washing step with demineralized water may involve, after the preceding steps, the extraction of the demineralized water inside the tank 20, the insertion of a second predetermined quantity of demineralized water inside the tank 20 and also comprises the following series of steps: activating a forced circulation continuously of the demineralized water for a time interval of between 3 and 7 minutes in the absence of an active electric field; interrupting the forced circulation; switching on the voltage generator 30 and activating an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; and switching off the voltage generator 30 in order to deactivate the electric field.
According to a particularly advantageous characteristic feature, during this treatment step the containers 40 containing the natural zeolite 1 may be placed close to the positive pole 32.
According to one of the embodiments of the present invention, at the end of the second washing step, the method may comprise a step of recovery and drying of the activated natural zeolite 1 . This step may comprise the steps of: extracting the demineralized water from the tank 20; extracting the activated natural zeolite 1 from the containers 40, and drying the natural zeolite 1 by means of a heat source.
The aim of this last step is to reduce the moisture in the mineral after activation until it falls to below 10%. This step is particularly useful in view of the fact that the natural zeolite 1 is a porous mineral.
According to another embodiment of the present invention, the activation method comprises a step of storing the activated natural zeolite 1 , during which the activated natural zeolite 1 is stored in air-free containers.
The activated zeolite 1 may then be packaged and remains stable and activated for a long period owing to the method of the present invention. The tests conducted hitherto have shown that the activated natural zeolite 1 remains fully stable for thirty- six months after the treatment if the product thus obtained has been properly stored.
The various research and development activities currently performed by the Proprietor have shown how the application of a very specific type of natural zeolite is able to heighten the performance of the natural zeolite activated according to the method of the present invention during the subsequent applications. In particular it has been found, from the current research and development activities, that a predetermined particle size is able to optimize the activation method. More
specifically it has been discovered that a particular particle size of natural zeolite 1 is correlated firstly to a specific porosity and at the same time to a well-defined physical-chemical structure thereof.
According to a particularly advantageous characteristic feature of the present invention, the natural zeolite 1 used in the activation method is of the LTA type and in the specific particle size to be applied it is characterized by an aluminium and silicon ratio of 1 , whereby single units form a meshwork formed by rings structured with six and four tetrahedrons joined together to form a structure similar to an octahedron. This structure provides the natural zeolite 1 with an average porosity of between 3.2 A and 4.8 A.
This aspect, related to a specific particle size, is of great importance since by using a predetermined type of natural zeolite which is characterized by uniform porosity associated with the treatment in a square wave electric field, a high standardization of the end product obtained is achieved, such that, in the various experiments carried out, the variability between the different batches is practically zero.
For this reason, according to a further embodiment of the present invention, the method for activation of natural zeolite 1 may also comprise a pre-treatment step which is performed before the first step for washing of the natural zeolite 1 . The aim of this step is to select the natural zeolite according to particle size so as to assign to the subsequent steps of the activation method only that quantity of natural zeolite which comprises a suitable predetermined stoichiometric structure.
The step for pre-treatment of the natural zeolite 1 comprises the steps of: screening natural zeolite 1 according to predetermined particle-size parameters, and separating the screened natural zeolite 1 from the rest of the natural zeolite.
This step of the method may also be performed in a separate location far from the location where the other steps of the activation method are performed. The fraction of natural zeolite 1 considered to be suitable is then transferred for the remaining steps of the method.
Numerous experiments carried out by the Proprietor have been able to define specific technical characteristics which allow identification of the activated natural zeolite 1 according to the present invention compared to a natural or synthetic zeolite which has not been activated.
For example, an electrolytic cell was prepared, said cell comprising a pair of electrodes each immersed at one of the two ends of a tank containing an electrolyte and a salt bridge via which the two electrolytic solutions were able to exchange ions. In particular, the electrolytic cell comprised a container 20, for example a tank, and a voltage generator 30. The pair of electrodes, i.e. two armatures 32, 34, were electrically connected to the two terminals of the voltage generator 30 so as to form, respectively, the positive pole 32 and the negative pole 34 of a dipole. The ratio between the distance of the electrodes 32, 34 inside the tank and their length was 8:1. The electrodes were made of a conductive material chosen from the group of materials comprising: metal alloys, copper, zinc, platinum, graphite or carbon. The temperature value of the electrolyte before the start of the experiments and in general of the surrounding environment was between 20 and 24°C.
In the various tests carried out, the electrolyte was formed by a phosphate buffer solution (KH2PO4), with a concentration of between 0.1 M and 0.5 M per litre.
Via the voltage generator 30 electric energy was supplied to the electrolytic cell in the form of an electric current. In the various tests carried out, the current had a voltage value of between 60 V and 100 V and a maximum amperage value of less than 16 A.
The experiments were carried out by introducing into the electrolytic cell first an activated natural zeolite 1 according to the present invention and then a zeolite which had not been treated. The values of the current output from the zeolite were measured by means of an ammeter able to cover the electric field concerned.
It was noted that the activated natural zeolite 1 offered greater resistance to the passage of electrons than the zeolite which had not been treated.
In particular, after a predetermined initial time interval from application of the electric energy to the electrolytic cell, for example, but not exclusively, after an interval of about 10 seconds, the activated natural zeolite 1 was able to reduce the current flow by an amount equal to between 35-45% of the current applied. After the same time interval, the zeolite which had not activated reduced the current value by an amount equal to not more than 18% of the current applied.
In one of the tests carried out with a concentration of the phosphate buffer solution equal to 0.3 M per litre and an applied current value equal to 80V, the reduction of the current flow was equal to 40% of the current applied.
Similarly, after a time interval of about 50-60 seconds from application of the electric energy to the electrolytic cell, the activated natural zeolite 1 reduced the current flow by an amount equal to between 12-14% of the current applied. After the same time interval, no reduction in the current flow through the zeolite which had not been activated was recorded.
From the results obtained it can be seen how the activated natural zeolite 1 according to the present invention acts a much more efficient resistor than the zeolite which had not been treated, namely it has a much higher electrical resistance action than that of zeolite which has not been treated.
The experimental tests were carried out using activated natural zeolite 1 with a predetermined particle size, for example with a value of between 0.5-1 .5 mm. Further tests carried out on zeolite with different particle sizes produced results showing a reduction of the current flow by different absolute amounts, but with percentages comparable with the aforementioned data, and with a different behaviour of the activated natural zeolite 1 and the non-activated natural zeolite as indicated above.
Among the numerous uses of the activated natural zeolite 1 , namely the natural zeolite 1 treated according to the preparation method described here, the Proprietor identified how the modification of the polar state of the natural zeolite 1 performed during the course of the method also produces a specific action thereof when it is added to a beverage. This action consists in an increase in the antagonistic activity against the free radicals present in the beverage. This aspect is the result of laboratory experiments aimed at providing a beverage with a "health-promoting" action.
The laboratory data obtained by the Proprietor has shown how the beverages obtained with the direct application of pre-treated natural zeolite and with a process for preparing the juice which directly involves the application of the activated natural zeolite 1 have the capacity to reduce the free radicals which is 30 to 32% greater compared to the action produced by a beverage obtained with the same composition, but with the application of non-activated zeolite, i.e. zeolite which has not been subjected to the method according to the present invention. This shows how the present method for activation of natural zeolite results in a substantial increase in the action which the mineral has once added to the preparation of the beverage.
This data undoubtedly constitutes an innovative feature since never before has this characteristic with its potential benefits been identified and described. It should be
pointed out that the action performed by the natural zeolite added during the preparation of a beverage, owing to its characteristics and the functions which it performs, also provides the beverage with an improved stability.
As described in the composition of the end product, the natural zeolite is applied in a maximum amount equal to 1%. More specifically, the mineral used is activated natural zeolite which has an "active mineral" action not only in connection with its chemical-physical characteristics - which are well-known and have been fully described - but also in connection with the treatment carried out on the natural zeolite in order to make it "active", this being then applied to the process for manufacture of the functionalized beverage which is characterized by an improved "healthpromoting" activity. All these characteristics have initially drawn attention to and at the same time resulted in the development of a biological process which may be used in the production of beverages of plant origin (fruit and vegetables in particular); these beverages are characterized by a high nutraceutical value resulting both from the metabolic potential of the raw material used and the innovative manufacturing process, which involves the addition of activated natural zeolite 1 , aimed at providing a series of products which may be characterized as being "health-promoting" and having a high nutraceutical value.
Only by way of example, the results obtained by applying the natural zeolite activated according to the method described to bergamot and apple juice are reported below: More specifically, activated natural zeolite was added in amount equal to 1% and the anti-radical activity was assessed by means of an assay of the DPPH (1 ,1 -diphenyl- 2-picrylhydrazyl).
The DPPH "scavenging assay" test is an assay used to determine the anti-radical activity in vitro. It is an accurate and highly reproducible assay based on the
discolouration of the DPPH (Blois 1958) which has deep purple colour with specific absorbance at 515-520 nm. In the presence of free radicals, DPPH turns pale yellow and the extent of discolouration is proportional to the anti-radical activity exerted by the matrix under analysis in relation to the DPPH. The extent of the anti-radical activity is assessed by spectrophotometric analysis at a wavelength of 517 nm.
More specifically, quantities of 50%-diluted apple and bergamot juice (indicated as MO and BO, respectively), to which natural zeolite 1 activated according to the method of the present invention was added in an amount of 1%, were analysed in triplicate by means of the DPPH test, obtaining two new compounds indicated as B1 and M1 , respectively.
In the comparative analysis conducted, quantities of juice in the same concentrations without the addition of activated natural zeolite 1 were analysed. The anti-radical activity was evaluated on the treated samples B1 , M1 , and on the untreated samples BO, MO, by spectrophotometric reading at 517 nm, at increasing time intervals following the addition of activated natural zeolite, where Ti = 1 h, T2 = 3h and T3 = 5h. The results obtained, shown in the graph in Figure 2, showed an improvement in the anti-radical activity exerted by the juice with the addition of natural zeolite, estimated at an average value for both juices of +30-32% compared to the juice without the addition of activated natural zeolite.
Another particularly effective application of activated natural zeolite 1 according to the present invention was also noted in the field of sanitary protection devices. A predetermined amount of activated natural zeolite 1 was added to the material used for the manufacture of filtering face-masks, i.e., sanitary masks. For example, in the case of masks made of non-woven fabric (Nwf), activated natural zeolite 1 was added to the polyester or polypropylene microfibres forming the filtering layer. The
results of the experiments carried out showed how the use of activated zeolite 1 contributed significantly to the reduction of the bacterial load filtered by the mask.
All the details may be replaced by other technically equivalent elements. Similarly, the materials used, and the associated forms and dimensions may be of any kind depending on the requirements, without thereby departing from the scope of protection of the following claims.
Claims
1 . Activated natural zeolite to be used for the conditioning of materials and/or substances, characterized in that it is able to reduce by a value of between 35% and 40% a current flow that passes through it when the activated natural zeolite is inserted in an electrolytic cell, within an initial time interval of 10 seconds from the application to said electrolytic cell of an electric current with a voltage value of between 60 V and 100 V, and a maximum amperage value of less than 16 A, said electrolytic cell comprising a container (20) and a pair of armatures (32, 34) arranged inside the container, the armatures (32, 34) being connected to a voltage generator (30) able to supply said current, said container (20) containing a phosphate buffer solution (KH2PO4), with a concentration of between 0.1 M and 0.5 M per litre.
2. Method for obtaining activated zeolite according to claim 1 , comprising the steps of subjecting natural zeolite (1):
- to a washing treatment with a mild saline solution and to an electric field with a square wave current flow for a predetermined time interval,
- to a first treatment with a sulphate buffer solution having an acidity value of between 5 and 6 pH and to an electric field with a square wave current flow for a predetermined time interval,
- to a second treatment with a phosphate buffer solution having an acidity value of between 5.5 and 6.7 pH and to an electric field with a square wave current flow for a predetermined time interval,
- to a third treatment with a phosphate buffer solution having an acidity value of between 6.5 and 7.5 pH and to an electric field with a square wave current flow for a predetermined time interval, and
24
- to a washing treatment with demineralized water and to an electric field with a square wave current flow for a predetermined time interval.
3. Method according to claim 2, characterized in that the washing treatment step with a mild saline solution comprises the following steps:
- subjecting the natural zeolite (1) to a forced circulation of the mild saline solution continuously for a time interval of between 5 and 10 minutes in the absence of an active electric field;
- interrupting the forced circulation of the mild saline solution;
- subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 8 and 12 minutes;
- deactivating the electric field, and
- subjecting the natural zeolite (1 ) to a forced circulation of the mild saline solution for a time interval of between 4 and 8 minutes.
4. Method according to claim 2, characterized in that the first treatment step with sulphate buffer solution comprises the steps of:
- subjecting the natural zeolite (1) to a forced circulation of the buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field;
- interrupting the forced circulation of the buffer solution;
- subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 3 and 7 minutes;
- deactivating the electric field; and
- subjecting the natural zeolite (1) to a forced circulation of the buffer solution continuously for a time interval of between 1 and 5 minutes.
5. Method according to claim 2, characterized in that the second treatment step with phosphate buffer solution comprises the steps of:
- subjecting the natural zeolite (1) to a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes in the absence of an active electric field;
- interrupting the forced circulation of the phosphate buffer solution;
- subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 6 and 10 minutes;
- deactivating the electric field; and
- subjecting the natural zeolite (1) to a forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes.
6. Method according to claim 2, characterized in that the third treatment step with phosphate buffer solution comprises the steps of:
- subjecting the natural zeolite (1 ) to a first forced circulation of the buffer solution continuously for a time interval of between 1 and 6 minutes in the absence of an active electric field;
- interrupting the first forced circulation of the phosphate buffer solution;
- subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 8 and 12 minutes;
- deactivating the electric field, and
- subjecting the natural zeolite (1) to a second forced circulation of the phosphate buffer solution continuously for a time interval of between 1 and 5 minutes;
- interrupting the second forced circulation of the phosphate buffer solution;
- subjecting the natural zeolite (1 ) to a third forced circulation of the phosphate buffer solution continuously for a time interval of between 4 and 8 minutes;
- interrupting the third forced circulation of the phosphate buffer solution;
- subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 12 and 18 minutes;
- deactivating the electric field.
7. Method according to claim 2, characterized in that the washing step with demineralized water comprises at least the steps of:
- subjecting the natural zeolite (1) to a continuous forced circulation of a first predetermined quantity of demineralized water for a time interval of between 3 and 7 minutes in the absence of an active electric field;
- deactivating the forced circulation and subjecting the natural zeolite (1) to an electric field with a square wave current flow for a time interval of between 6 and 10 minutes; and
- deactivating the electric field.
8. Method according to claim 7, characterized in that it further comprises a step of storing the natural zeolite (1) in an air-free environment.
9. Method according to claim 2, characterized in that before the first step of washing the natural zeolite with a mild saline solution it also comprises a pretreatment step, comprising the steps of:
- screening the natural zeolite (1 ) according to its particle size, and
- separating the screened natural zeolite (1) from the rest of the natural zeolite.
10. Method according to claim 2, characterized in that it comprises the steps of preparing:
- a container (20),
- a voltage generator (30), and
27
- two armatures (32, 34) arranged at the two ends of the tank (20) and electrically connected to the two terminals of the voltage generator (30) so as to form, respectively, the positive pole (32) and the negative pole (34) of a dipole, and placing the natural zeolite (1) inside the container (20).
1 1 . Method according to claim 10, characterized in that:
- during the washing step with mild saline solution the natural zeolite (1 ) is placed at the positive pole (32),
- during the first treatment step with a sulphate buffer solution the natural zeolite (1) is placed at the negative pole (34),
- during the second treatment step with a phosphate buffer solution the natural zeolite (1) is placed at the negative pole (34),
- during the third treatment step with a phosphate buffer solution, the natural zeolite (1 ) is placed at the negative pole (34), and
- during the washing step with demineralized water, the natural zeolite (1) is placed at the positive pole (32).
28
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105314704A (en) * | 2014-07-11 | 2016-02-10 | 上海博丹环境工程技术股份有限公司 | Ammonia-nitrogen wastewater processing method and system, and sodium modified zeolite regeneration method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314704A (en) * | 2014-07-11 | 2016-02-10 | 上海博丹环境工程技术股份有限公司 | Ammonia-nitrogen wastewater processing method and system, and sodium modified zeolite regeneration method |
Non-Patent Citations (2)
| Title |
|---|
| LEI X ET AL: "Electrochemical regeneration of zeolites and the removal of ammonia", JOURNAL OF HAZARDOUS MATERIALS, ELSEVIER, AMSTERDAM, NL, vol. 169, no. 1-3, 30 September 2009 (2009-09-30), pages 746 - 750, XP026282729, ISSN: 0304-3894, [retrieved on 20090409], DOI: 10.1016/J.JHAZMAT.2009.04.012 * |
| LI M ET AL: "Application of an electrochemical-ion exchange reactor for ammonia removal", ELECTROCHIMICA ACTA, ELSEVIER, AMSTERDAM, NL, vol. 55, no. 1, 15 December 2009 (2009-12-15), pages 159 - 164, XP026670107, ISSN: 0013-4686, [retrieved on 20090825], DOI: 10.1016/J.ELECTACTA.2009.08.027 * |
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