• 专利附录
  • 专利说明
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    • 专利摘要:
    Indicator ink of the freshness of food and procedure for the manufacture of an ink indicating the freshness of food. It comprises between 90-98% of the total, a varnish, said varnish comprising between 5-25% of the total varnish of at least one film-forming resin or at least one vinyl resin or a mixture thereof, between 10-25 % on the amount of resin of a plasticizer additive and between 50-75% of the total solvent varnish, and between 2-10% of the total, some metal salts. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2540786A1
    申请号:ES201430022
    申请日:2014-01-10
    公开日:2015-07-13
    发明作者:Ugo La Valle Sansone；Antonio López Muñoz；Emilio FERNÁNDEZ GARCÍA；Joaquín CORTIELLA MARTORELL；Núria HERRANZ SOLANA；Inmaculada LORENTE GÓMEZ；Teresa CALVO VILANOVA；Susana Aucejo Romero；Ramón Martínez Mañez；José Luis VIVANCOS BONO；Patricia ZARAGOZA TORRES；José VICENTE ROS LIS
    申请人:Instituto Tecnologico Del Embalaje Transporte Y Logistica；INST TECNOLOGICO DEL EMBALAJE TRANSPORTE Y LOGISTICA；Universidad Politecnica de Valencia；Chimigraf Iberica SL；
    IPC主号:
    专利说明:

    2DESCRIPTION Food freshness indicator ink and procedure for manufacturing a food freshness indicator ink.5 Food freshness indicator ink and procedure for the manufacture of a food freshness indicator ink, in particular for those foods that degradation process emit sulfur compounds such as hydrogen sulfide, dimethyl sulphide, dimethyl disulfide, 2,3-dimethyl trisulfide, thiols such as methanethiol, ethanethiol, or the like, and comprising: between 90-98% of the total, a varnish, comprising said varnish, between 105-25% of the total varnish of at least one film-forming resin or at least one vinyl resin or a mixture thereof, between 10-25% on the amount of resin of a plasticizer additive and between 50- 75% of the total solvent varnish, and between 2-10% of the total, metal salts. 15 BACKGROUND OF THE INVENTION Different inks are known in the state of the art that change the color before the change of state of food.20 Thus, it belongs to the state of the art, German Patent No. 19605522, of the year 1996, in the name of KARLSRUHE FORSCHZENT that It refers to a layer sensitive to an optochemical sensor that has a phthalocyanine metal complex fixed in a porous matrix. Also known as European Patent No. 0449798, in the name of AVL MEDICAL 25INTRUMENTS, from 1991, which refers to To control the quality of the packages of organic substances, preferably of packaged food products, tea, coffee, tobacco and medicines, the substances to be examined are put in contact with a planar optical sensor element that is mounted inside the packing and this reacts to the change in the composition of the gas in the space above the sample by a change in color or fluorescence. The change in one of the optical properties of the sensor element is detected visually or optoelectronically. There are also other patents that can be considered as US2006057022 “FOODQUALITY INDICATOR”, of 2005, which refers to an indicator that uses 35P20143002210-01-20143 natural pH indicators and reacts against acids, such as H2S. It is an indicator that cannot be used in a modified atmosphere. Within the same group we find the Patent WO2011045572 “INTELLIGENT PIGMENTS AND PLASTICS”, of the year 2010, which refers to an indicator such as polymer 5composite through melt processing, which is used for use in food packaging, which is sensitive to CO2, O2 and NH3, with indicators such as m-cresol purpple, bromopheol blue, methylene blue, etc., being said dye or ink by coating or impregnation with inorganic pigments such as SiO2TiO2 , Al2O3, MgO, zeolites, which ultimately gives a water soluble ink. When CO2 is used, this indicator cannot be used in a modified atmosphere. Thus, WO2009 / 070760 "HYDROGEN SULFIDE INDICATING PIGMENTS", of 2008, refers to pigments that react to hydrogen sulfide, with application to environmental safety. It is known that metals react to hydrogen sulfide by changing color, however the color change does not occur gradually or directly linked to the concentration of food spoilage compounds in contracted atmospheres inside the container of fresh produce. Background US Patent No. 7153532, in the name of JOHNSON MATTHEY PLC, 20 of the year 2001, which refers to a sensor for the detection of food spoilage or the opening or breakage of the packaging, which comprises a metal complex fixed in or on a substrate, whose complex is capable of releasing a detectable component.BREVE DESCRIPTION OF THE INVENTION25The present invention is an improvement in the sector of the inks that change the color before the degradation or decrease of the freshness of the food and the processes for the manufacture of The same.30 At present, quality and safety are the fundamental priorities for the food industry a and the authorities, and that is why the current lines of research in Europe are aimed precisely at ensuring quality and safety in food.35P20143002210-01-20144As is logical, the packaging systems that contain and protect food throughout its useful life are subject to this same trend. In particular, the primary packaging, which constitutes a vital element to ensure the quality and safety of the packaged product, plays a crucial role in achieving this objective. 5On the other hand, it has been detected that the quantity of products discarded along the supply chain, and that they could actually be consumed without problems, is worryingly high.The ability to have a system that individually, non-destructively and Real-time report on food quality and safety is a complementary and valuable tool to achieve the objectives set by the European Union. Currently, the expiration date is set based on the production date, so that the first thing that is produced is the first thing that should be consumed, without taking into account the storage conditions or the initial microbial load of the product , which causes that sometimes product is discarded that could really be consumed in perfect conditions, or that poisonings occur due to the consumption of product in poor condition. 20In this situation, and with the aim of ensuring the quality and safety of food and reducing the amount of wasted food, the present invention provides information on the shelf life of the food in real time, based on aspects of the product, such as for example, its microbial load or physical-chemical characteristics, and not in the currently used estimating methods that do not take into account possible breaks in the cold chain. The closest document is the cited US patent No. 7153532.This document mainly solves the detection of degree of freshness in foods packaged using an ink composition comprising indicator compounds, resins, solvents and additives. Thus, the change in optical properties is experienced by chromophores and / or fluorophores attached to the metal center, showing a color change and a fluorescence change when the product is expired. 35P20143002210-01-20145In addition, some of the elements used as titanium or rare earth are not very suitable for packaging food with low cost of sale, since its cost does not compensate for the economic cost of the product.Finally, the aforementioned document has the following limitations: 5- It requires an optical element for viewing, and -the developed indicator includes a metal complex whose manufacturing process on an industrial scale is not defined or optimized.10 The present invention improves the closest document since the ink obtained in the process does not require of optical elements for visualization (fluorescence change), so that anyone with the naked eye can realize the degree of freshness of the food that is sold, in addition the color change is experienced by the metal itself without the need to form complexes with groups Photoactive, it is much more precise in 15 the change of colorya that is totally in line with the deterioration of the food and much more economical to obtain. Finally, the following advantages are worth mentioning: 20-All the materials used in the manufacture of the indicator are suitable for food contact or also known as “food contact”, because they are contrasted with the positive lists and legislation of materials Suitable for food contact.-In addition, the materials used are economical materials, so the cost of their development can be borne by low-priced food products.-Irreversible change: in case the package is broken and the composition is modified gaseous inside, the indicator will not revert to its initial coloration, so it will not show a false positive. All this makes the present invention suitable for the packaging of food products that emit sulfur compounds in their degradation process.It is an object of the present invention an ink indicating the freshness of food, in particular for those foods that in their degradation process emit sulfur compounds such as hydrogen sulfide, dimethyl sulfide, dimethyl disulfide, 2,3-dimethyl trisulfide, P20143002210-01-20146 thiols such as methanethiol, ethanothiol, or the like, characterized in that it comprises: between 90-98% of the total, a varnish, said varnish comprising, between 5-25% of the total varnish of at least one film-forming resin or at least one vinyl resin or a mixture thereof, between 10-25% on the amount of resin of a plasticizer additive and between 50-75% of the total solvent varnish, and between 2-10% of the total, metal salts. 5It is a further object of the invention a process for the manufacture of an ink indicating the freshness of food, in particular for those foods that in their degradation process emit sulfur compounds such as hydrogen sulfide, dimethyl sulphide, dimethyl disulphide, 2,3 - dimethyl trisulfide, thiols such as methanethiol, ethanothiol, or the like, of the type characterized in that it comprises: a first phase in which a varnish is prepared by adding at least one resin, vinyl or at least one film-forming resin or a mixture Of these, and with at least one plasticizer additive compatible with the resin and added to a mixture of solvents and stirred until its total solubility, the resin being between 5-25% of the total, the plasticizer additive between 10- 25% on the amount of resin and the solvents between 50-75% of the total, a second phase in which a concentrated base ink formed by the varnish obtained by adding the previous phase and a metal salt, said metal salt (indicator) is prepared in Slow stirring in the varnish, all of which is subsequently agitated and defining a concentrated base ink, the metal salts being between 15-30% of the total ink and the varnish between 70 -85%, a third phase in which the dispersion from the previous phase it is milled in a microsphere mill until a uniform granulometry dispersion of less than 5µ is obtained, and a fourth phase in which this concentrated base ink is diluted in the varnish manufactured in the first phase, until Concentration of metallic salt between 2 and 10% of the total weight of the ink. 25 BRIEF DESCRIPTION OF THE DRAWINGS In order to facilitate the explanation, three sheets of drawings in which a practical case of embodiment has been represented are attached. which is cited by way of example, not limiting the scope of the present invention: 30 "Figure 1 is a graph of the average color differences of indicators evaluated as a function of time and with respect to their initial color." Figures 2 and 4, are two possible designs that the indicator can present. IguraFigure 3 and 5, are profile views of figures 1 and 3 and show the structure of the indicator. P20143002210-01-20147 CONCRETE EMBODIMENT OF THE PRESENT INVENTION Thus, in a specific embodiment, the process for the manufacture of an ink indicating the freshness of food, such as poultry, pork or beef, which in its degradation process emit compounds Sulfur compounds such as hydrogen sulfide, dimethyl sulphide, dimethyl disulfide, 2,3-dimethyl trisulfide, thiols such as methanethiol, ethanethiol, etc., comprise the following phases: A first phase in which a varnish is prepared by adding a resin derived from the 10 cellulose or a mixture thereof, such as ethyl cellulose, cellulose acetopropionate, nitrocellulose, as well as vinyl resins and other similar film-forming resins. In this embodiment, an alcohol-wetted nitrocellulose is used, such as 65% by weight nitrocellulose (content N <12.3%) moistened in ¼ viscosity isopropyl alcohol having good solubility in a mixture of ethyl alcohol and acetate Ethyl, although other resins derived from cellulose such as ethyl cellulose, cellulose acetopropionate, etc. could also be thought of. The above resin is plasticized with at least one plasticizer additive compatible with the cellulose derived resin. In this embodiment, acetyl tributyl citrate is used. The plastification is carried out because the resins derived from cellulose when printing form rigid and fragile films, hence it is plasticized with acetyl tributyl citrate to give it greater flexibility. The resulting mixture is added to a solvent mixture and the solubility is stirred to a total of 600 rpm. Depending on the printing process (flexography, rotogravure, inkjet, ...) it will be formulated with the most suitable solvents (ethyl alcohol, ethyl acetate, n-propyl acetate, methoxypropanol, ethoxypropanol, ...) taking into account factors such as the solubility of the resin, the rate of evaporation, the tendency to be retained in the support, its null or low harmfulness, etc. 30 So a base composition would be formed by the cellulose-derived resin between 5-25% of the total, the plasticizer additive between 10-25% on the amount of resin and solvents between 50-75% of the total, which would be specified in an example as follows: 35 ° Nitrocellulose (65% solids): 20% P20143002210-01-20148  Acetyl tributyl citrate: 5%  Ethyl alcohol 99.8º: 60%  Ethyl acetate: 15% The viscosity of the varnish measured in Ford Cup No. 4 (CFN4) is 25 ”-40” at 20ºC. 5 Next in second phase in which it prepares a concentrated base ink formed by the varnish obtained in the previous phase and a metal salt.The metal salts (indicator) can be, for example, copper salts or iron salts, specifically copper carbonate and nitrate of iron.The metallic salt (indicator) is added by adding it in slow agitation in the varnish, and stirring all this later, for example at 1200 rpm for 15 minutes, and defining a concentrated base ink, the metal salts being between 2-10% of the total 15 of the ink and varnish between 90-98%. An example of formulation could be:  Copper salt: 10% 20  Varnish: 90% In the third phase in which the dispersion of the previous phase is ground with microspheres , for example Zirconium Oxide / Yt River between 0.6mm -1.2mm in diameter, until a uniform granulometry dispersion of less than 5µ.25 is obtained. It is recirculated for a minimum of 30 min in the microsphere mill. A uniform granulometry dispersion of pale bluish-greenish color (in the case of copper salt) and dark brown color (in the case of iron salt) is obtained. The viscosity of the base ink measured in Ford Cup No. 4 (CFN4) is 25 ”-50” at 20 ° C. 30 Finally, in the fourth phase, the concentrated base ink, obtained in the third phase, is diluted with the varnish manufactured in the first phase, up to a concentration of metallic salt between 2 and 10% of the total weight of the ink. 35P20143002210-01-20149 Thus, the ink indicating the freshness of poultry meat object of the present invention would comprise: 90-98% varnish 2-10% metal salts5 The varnish, in turn, comprises: -255-25% of the total of varnish of a resin derived from cellulose, -2510-25% on the amount of resin of a plasticizer additive, and 1050-75% of the total solvent varnish.In this embodiment a nitrocellulose moistened in alcohol or in another solvent compatible with the formulation, such as nitrocellulose (content N <12.3%) at 65% by weight moistened in ¼ viscosity isopropyl alcohol having good solubility in mixture of ethyl alcohol and ethyl acetate, but also One could think of other cellulose-derived resins such as ethyl cellulose, cellulose aceto-propyanate, vinyl resins and other similar film-forming resins. The plasticizer additive has to be compatible with the cellulose-derived resin. In this embodiment, acetyl tributyl citrate is used. The plasticization is done because nitrocellulose when printing forms rigid and fragile films, hence it is plasticized with acetyl tributyl citrate to give it greater flexibility. Depending on the printing process (flexography, gravure, inkjet, ...) it will be formulated with solvents more suitable, taking into account factors such as the solubility of the resin, the rate of evaporation, the tendency to be retained in the support, its null or low harmfulness, etc. An example of varnish would be the following: 30 ° Nitrocellulose (65% solids): 20%  Acetyl tributyl citrate: 5%  Ethyl alcohol 99.8º: 60%  Ethyl acetate: 15% 35P20143002210-01-201410% are by weight in relation to the total referenced. The viscosity of the varnish measured in Ford Cup No. 4 (CFN4) is 25 "-40" at 20 ° C. 5 As regards metal salts, these can be copper or of iron, for example.It is an indicator ink that contains an indicator compound in its formulation, metallic salt. Once the indicator ink has been manufactured by the process explained above, it is printed on a porous substrate, for example paper and cardboard of different qualities, suitable for food contact and permeable to volatile compounds but impervious to the passage of the ink components to the packaged product, subsequently a strip is printed with the reference colors indicative of the state of degradation. This impression is adhesive to be able to be adhered by the inner side of the containers, for example by the inner side of the sealing films of wafers with product.The food is degraded by different processes: physical, chemical, biological, environmental, etc. In the case of packaged foods, degradation by physical processes (blows) is minimal and degradation is mainly due to the growth of microorganisms, which can be favored if environmental conditions (temperature) are not adequate. During the shelf life of food, these microorganisms grow and multiply at the expense of the product itself, modifying its sensory characteristics and generating volatile compounds, for example volatile sulfur compounds, which are accumulated in the head space of the container. The shorter the shelf life of the food, the greater the concentration of 25 volatile compounds in the head space of the container. These compounds pass through the porous substrate on which the indicator ink is applied, reacting with the metal salt and causing a change in their coloration. This change is proportional to the concentration of volatile sulfur compounds in the head space of the container, and therefore It is related to the shelf life of the packaged product. This indicator also has a legend in which it is explained to which useful life each color of the indicator ink corresponds, so that the consumer when using it does not have doubts about the information that the indicator shows.35P20143002210-01-201411The printing methods are traditional printing systems (flexography, gravure, inkjet, ...) used in label printing and known to experts in the field. Finally, all printing is protected with a support material (for example non-stick silicone paper) .For the use of the indicator ink in the indicator, the described freshness ink is printed on a porous substrate permeable to volatile compounds. Printing used can be flexography, gravure, inkjet, etc., obtaining a dry layer thickness between 0.05 and 3 microns. Subsequently, the indicator legend is printed with all the information necessary for the interpretation of the color of the indicator. A layer of adhesive is then printed and the printing is protected with a support material (for example non-stick silicone paper). This indicator is adhered on the inside of the sealing film of a boat that contains, for example, poultry meat packaged in a modified atmosphere, for example 1570% CO2 and 30% N2. The boat with the indicator is stored at a cooling temperature of 4ºC. After performing sensory analysis (visual evaluation and olfactory evaluation) and microbiological (total aerobic, Enterobacteria and Salmonella), it is determined that the product reaches the end of its useful life between 9 and 15 days of packaging. In an example in which a shelf life of 9 days was obtained, the average color of the indicator on day 0 of packaging is L = 91.8; a = -2.44; b = 5.91. The average color of the indicator on day 9 of packaging is L = 78.80; a = 0.99; b = 11.32. The average color difference between the initial color of the indicator and the final color is 14.5 (Fig. 1). As can be seen in figure 1, the color change occurs gradually, according to the deterioration of the food. Illustrative and exemplary, four figures are attached that explain a little more visually the changes that users could observe depending on the useful life of the food. Figures 2 and 4 are two possible designs that the indicator can present. One as in Figure 2 based on a disk (1) and in Figure 4 to a strip (41), which would be attached inside the package, in the film thereof for example.35P20143002210-01-201412 Both the disc (1) and the strip (41) are divided into four cells, for the disc (2,3,4,5), for the strip (42,43,44,45) that define a color depending on the degradation of the food and the emission of sulfur compounds, the ink impregnates the porous substrate (6.46). Thus, if the food had a shelf life of 3 days the color would be like that of the cells5 (2.42), if it were 4 to 7days it would change its color like that of the cells (3.43), if it already reached the useful AIDS of more than one week the color would be like that of the cells (4.44) and finally if its consumption was not already advised by the state of degradation , its color would be like that of the last cells (5.45) .10 In Figures 3 and 5, which are sections of the respective 2 and 4, and showing the structure of the indicator, the placement of the indicator ink can also be seen (8.48), as well as the transparent adhesive (7.47). The present invention patent describes a new indicator of freshness of foods and processes dimiento for the manufacture of an ink indicating the freshness of food. The examples mentioned herein are not limiting of the present invention, therefore it may have different applications and / or adaptations, all of them within the scope of the following claims.20P20143002210-01-2014
    权利要求:
    Claims (1)
    [1]
    13 CLAIMS 1. Food freshness indicator ink, in particular for those foods that in their degradation process emit sulfur compounds such as hydrogen sulfide, dimethyl sulfide, dimethyl disulfide, 2,3-5 dimethyl trisulfide, thiols such as methanethiol, ethanethiol , or the like, characterized in that it comprises: - between 90-98% of the total, a varnish, said varnish comprising, between 5-25% of the total varnish of at least one film-forming resin or 10 at least one vinyl resin or a mixing them, between 10-25% on the amount of resin of a plasticizer additive and between 50-75% of the total solvent varnish, and - between 2-10% of the total, metal salts. 2. Ink, according to claim 1, characterized in that the viscosity of the base ink measured in Ford Cup No. 4 (CFN4) is 25 "-50" at 20 ° C. 3. Ink according to claim 1, characterized in that the resin is a resin derived from cellulose. Ink, according to claim 3, characterized in that the cellulose-derived resin is a wetted nitrocellulose. 5. Ink according to claim 3, characterized in that the cellulose-derived resin is an ethyl cellulose. 6. Ink according to claim 3, characterized in that the cellulose-derived resin is a cellulose aceto-propyanate. 7. Ink, according to claim 1, characterized in that the solvent is ethyl alcohol and ethyl acetate. 8. Ink according to claims 4 or 5 or 6, characterized in that the plasticizer additive is acetyl tributyl citrate. 3514. Ink, according to claim 1, characterized in that the metal salts are copper salts. 10. Ink according to claim 1, characterized in that the metal salts are iron salts. 11. Ink according to any of the preceding claims, characterized in that the viscosity of the varnish measured in Ford Cup No. 4 (CFN4) is 25 "-40" at 20 ° C. 10 12. Process for the manufacture of an ink indicating the freshness of food, in particular for those foods that in their degradation process emit sulfur compounds such as hydrogen sulfide, dimethyl sulphide, dimethyl disulfide, 2,3-dimethyl trisulfide, thiols such as methanethiol, ethanothiol, or the like, of the type characterized in that it comprises: - a first phase in which a varnish is prepared by adding at least one resin, vinyl or at least one film-forming resin or a mixture 20 of them, and with at minus a plasticizer additive compatible with the resin and added to a mixture of solvents and stirred until its total solubility, the resin being between 5-25% of the total, the plasticizer additive between 10-25% on the amount of resin and the solvents between 50-75% of the total, 25 - a second phase in which a concentrated base ink formed by the varnish obtained by adding the previous phase and a metal salt is prepared, d icha metal salt (indicator) in slow agitation in the varnish, all of which is subsequently stirred and defining a concentrated base ink, the metal salts being between 15-30% of the total of 30 ink and varnish between 70-85%, - a third phase in which the dispersion of the previous phase is ground in a microsphere mill until a uniform particle size dispersion of less than 5µ is obtained, and15 - a fourth phase in which this concentrated base ink is diluted in the varnish manufactured in the first phase, to a concentration of metal salt between 2 and 10% of the total weight of the ink. 13. Method according to claim 12, characterized in that the resin is a resin derived from cellulose. 14. Method according to claim 13, characterized in that the cellulose-derived resin is a wetted nitrocellulose. 15. Process according to claim 13, characterized in that the cellulose-derived resin is an ethyl cellulose. 16. Process according to claim 13, characterized in that the cellulose-derived resin is a cellulose aceto-propyanate. 17. Process according to claim 12, characterized in that the solvent is a mixture of ethyl alcohol and ethyl acetate. 18. Method according to claims 14 or 15 or 16, characterized in that the plasticizer additive is acetyl tributyl citrate. 19. Method according to any of the preceding claims, characterized in that the mixture of the first phase is stirred at 600 rpm until completely soluble. 20. Method according to claim 12, characterized in that the metal salts of the second phase are copper salts. 21. Method according to claim 12, characterized in that the metal salts of the second phase are iron salts. 22. Method according to claim 12, characterized in that the stirring of the second phase is carried out at 1200 rpm for a minimum of 15 minutes. 3523. Method according to claim 12, characterized in that the homogeneous dispersion is carried out in a Zirconium / Ytrium Oxide microsphere mill for 30 minutes.
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