Classifications

• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23K—FODDER
  • A23K20/00—Accessory food factors for animal feeding-stuffs
  • A23K20/10—Organic substances
  • A23K20/179—Colouring agents, e.g. pigmenting or dyeing agents
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23K—FODDER
  • A23K40/00—Shaping or working-up of animal feeding-stuffs
  • A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
  • A23L5/40—Colouring or decolouring of foods
  • A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
  • C09B67/0092—Dyes in solid form
  • C09B67/0095—Process features in the making of granulates
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes

Definitions

• the present invention relates to the dyestuffs industry. It relates to the manufacture of dyes soluble in an aqueous medium, such as those in particular based on coloring compounds of organic nature, which are intended to be marketed in solid form for use in various industries for the coloring of aqueous vehicles.
• the dyes in question are used in particular in the food industry, where they are used to color food.
• Foods that are distributed industrially in the form of beverages are just one example, as there are many solid foods that are common to color in a similar fashion.
• these dyes are also used in the pharmaceutical industry and the cosmetic industry.
• the invention has the advantage of leading to non-toxic products, which are compatible with all the health requirements which must be met in the case of products intended for ingestion or absorption by humans. Similar requirements are met for animals, for farm animals in particular, so that the invention satisfies the same advantages in the context of the dyes that are used for animal feed, for example to distinguish by the color of different food compositions.
• the present invention proposes to present the dyes, in particular those intended for the food industry, in solid form in mixture with a binder essentially consisting of polyethylene glycol in which they are previously diluted at a temperature above the melting temperature of said binder.
• the mixture also comprises a component capable of manifesting an effervescent effect in the aqueous vehicle for which the dye is intended.
• This constituent, or effervescent agent is in practice a mixture of two compounds which are finely distributed individually in the final product, so as to be ready to react but only in the presence of water.
• the polyethylene glycol in the molten state is capable of dissolving without difficulty significant proportions of the chemical compounds constituting the organic dyes and that, in addition, with equal weight of dye compound , the solid product containing them in intimate mixture in the mass with the binder, as obtained after cooling, is endowed with a better solubility, or at least with a speed of dissolution in water and aqueous vehicles which is very significantly increased compared to the starting micron powder.
• an effervescent agent is adjusted to best improve the capacity of the finished product constituted by the mixture in the solid state to dissolve quickly in water and its nature is chosen to ensure its solubility in the binder in the effective proportion.
• an effervescent agent is advantageously chosen from combinations which generate carbonic acid which are recognized as non-toxic and acceptable in food.
• the typical example from this point of view is represented by a substantially stoichiometric mixture of citric acid and sodium carbonate, both of these compounds being easy to dissolve in the binder without the effervescent reaction occurring. as long as the mixture is not brought into contact with water.
• the subject of the invention is also a process for the production of coloring products, in particular so-called food coloring, intended in particular for the food industry, which is characterized in that it consists essentially in diluting a pulverulent coloring organic compound in a binder in fusion essentially consisting of polyethylene glycol advantageously in admixture with an effervescent agent, and in cooling the mixture obtained to obtain a dye in solid form in which the dye compound is intimately mixed with said binder.
• the method according to the invention meets various secondary characteristics, which can be applied individually or in any technically effective combination to result in a dye such as those which are also subject of the present invention, that is to say a dye product which is in solid form, not generating dirty dust, and soluble in aqueous vehicles.
• the starting coloring material is preferably initially in the form of a powder with micron particle size
• the polyethylene glycol is itself preferably used in the form of a powder
• both Powder components are advantageously dry mixed before heating the mixture to a temperature sufficient to ensure the melting of the binder.
• the polyethylene glycol is a polymer from the class of polyolefins which is used according to the invention in a quality corresponding to a relatively low polymerization rate, so that it is not only very soluble, but also fusible at a temperature below 120 ° C.
• the qualities of polyethylene glycol, or homologous compounds and equivalent derivatives, which allow the fusion to take place at a temperature between 40 ° C. and 80 ° C. are preferred. If only from an economic point of view, it is always advantageous to be able to be content with heating at lukewarm temperature, and moreover, any effect which would tend to degrade the coloring compound should be avoided. But on the other hand, it is desired to recover a solid product at ordinary temperature, also capable of withstanding variations in ambient temperature in the user factories.
• the invention encompasses the case where there is only apparent dissolution, each particle of micron dimension is found individually coated in the mass of the binder. This is also how it is usual in industrial practice to apply the term dye to mineral pigments when, by an ultra-fine particle size, their behavior is such that their dilution is comparable to a true dissolution. .
• the invention provides preferably from a pulverulent coloring compound with a particle size of less than 100 microns, advantageously of the order of 10 to 50 microns.
• Respecting a similar condition of very fine particle size is also desirable when it is planned to introduce the coloring compound directly into the binder already melted separately, which then takes the form of a viscous liquid.
• the polyethylene glycol is incorporated in divided form, in particular in the form of a powder with a particle size of on the order of a millimeter because economic factors (essentially in cost of the raw material) make grain sizes greater than 500 microns prefer.
• the proportions of the constituents used can be very variable, depending in particular on their respective physicochemical properties. They can also vary according to the dimensions desired for the final solid product. The latter will themselves be extremely variable, depending principally on each particular application case for which the product is intended. For example, for a dye which is in the solid state in a divided form, in particular for making a flowable product, consisting of granules or other similar elements and delivered in bulk, a composition less rich in polyethylene is advantageously provided. glycol than for a product that ultimately presents in bricks or other solid blocks requiring shaping by molding, possibly by extrusion.
• the product obtained according to the invention may advantageously contain a mixture of different coloring organic compounds, in order to lead to shades which can be chosen as desired. It is easily understood that in this case, it is advantageously up to the manufacturer implementing the method according to the invention to ensure the appropriate composition and thus to preserve the obtaining of the desired shade for a determined dosage. The user client no longer has to fear the consequences of errors or negligence in weighing the dose of each dye.
• the composition of the product of the invention comprises from 10 to 80% and, preferably, from 15 to 60% of polyethylene glycol relative to the total weight of the composition.
• the proportion of dye is advantageously between 10 and 70%, and preferably between 30 and 50%, relative to the total weight of the composition.
• the effervescent agent in ternary mixtures it is advantageously present in the proportion of 10 to 60% and, preferably, from 15 to 50% relative to the total weight of the composition. In all cases, whether or not the total composition comprises effervescent agent, it seems that the best results are obtained when the binary mixture of polyethylene glycol comprises from 0.5 to 1.5 parts by weight of poly- ethylene glycol for a part by weight of the starting coloring compound.
• the presentation in the form of granules in bulk the dimensions of which are advantageously between 0.2 and 10 millimeters, therefore overall on the order of a millimeter.
• Such granules can be obtained by precipitation directly from the molten mixture of the constituents.
• each element or block can advantageously constitute a dose of coloring product for a production batch of the aqueous vehicle in which it will be dissolved.
• an organic compound known as a synthetic dye is used as it is traditionally obtained in powder form, with micron particle size, by fluidization or micronization at the end of the industrial synthesis process.
• the binder used is commercial polyethylene glycol (PEG), in the form of granules with an average particle size of the order of 500 microns.
• PEG polyethylene glycol
• the composition includes an effervescent agent. This is prepared beforehand. It is composed of 64.5% citric acid and 35.5% sodium carbonate, both in crystalline form. These proportions correspond substantially to the stoichiometric equilibrium of the effervescent reaction between the two constituents.
• composition is made up by dry mixing of 40% by weight of E104 with 25% by weight of PEG and 35% by weight of effervescent agent (total of its two constituents).
• the powder mixture obtained is carefully heated until it is uniformly liquid. This is done in a water bath brought to the boil, therefore at a temperature close to 100 ° C.
• the melting point of the assembly is governed by the PEG at 54 ° C., and with regard to it, in the absence of moisture, the effervescent agent is inert in solution.
• the molten mixture is then cooled so as to ensure its precipitation in the form of solid granules, slightly pasty, which are collected and kept under moderate stirring until complete cooling to room temperature, in order to avoid that the granules agglomerate in blocks.
• the procedure is substantially as in the previous example, replacing the dye E104 by food coloring E102, that is to say tartrazine yellow, the chemical formula of which is a phenyi-azo-pyrazole trisodium carboxylate.
• the industrial powder is 85% pure and has a molecular weight of 534.4. It is an orange color which provides yellow in solution.
• composition is chosen at 40% of dye E1 02 for
• the mixture obtained is heated to a temperature of 70-80 ° C, at which it is maintained until a very homogeneous liquid product is obtained.
• its cooling is provided in the form of solid granules.
• the granules are sorted on a mesh size screen adapted to the desired particle size.
• the sieving is carried out in two or three stages intercalating with a crushing of the elements too large to pass through the meshes of the sieve, so as to finally obtain granules of substantially isotropic dimensions of the order of 0.5 to 1 millimeter in diameter.
• the product is weighed and delivered in bulk. It is particularly well suited for beverage manufacturers, since it is easy to dissolve in aqueous liquids by using the means of homogenization of materials already existing in factories for current dyes. Note that at equal concentrations, the yellow color of the base dye is in no way altered by the process according to the invention.
• the procedure is as in the previous examples for a composition comprising 40% by weight of dye E102 or E104 for 35% by weight of PEG and 25% by weight in total of the two constituents of the effervescent agent.
• the formation of the granules is carried out without difficulty. , avoiding a pasty consistency which could cause the formation of blocks which should then be crushed.
• the granules obtained have diameters less than 2 to 3 millimeters.
• a composition comprising 50 parts by weight of effervescent agent for 40 parts by weight of polyethylene glycol and 10 parts by weight of colorant. This naturally results in a lower coloring power, but the final shade of the dissolved product is preserved as soon as the dilution rate of the basic coloring is the same.
• the process thus implemented with granulation of the product during the cooling of the molten mixture leads to granules of dimensions of the order of a millimeter, which can advantageously vary between 0.2 mm and 10 mm in diameter.
• Dye E124 (culvert red) is used at a dose of 35% for 40% of PEG and 25% of effervescent agent.
• the still pasty mixture is shaped by extrusion through a die delivering a continuous wire with a diameter of around 2 mm which is immediately cut into elements the length of which is around of the centimeter.
• this length for example to values which can range from 0.5 to 20 millimeters, the dose of basic dye represented by each element can be adjusted.
• the homogeneous liquid obtained is cooled to a pasty state, at a temperature of the order of 40 to 50 ° C, and poured into molds from which it is extracted, after complete cooling, in the form of elements single dose.
• each pellet With molds leading to disc-shaped pellets 4 cm in diameter and 5 mm thick, the weight of each pellet is 10 g, which represents a coloring power corresponding to 3.5 g of basic dye.
• the procedure is as in one or other of the examples above, but starting from a composition in which the proportion of the dye is composed at 30% by weight of dye E132 (indigotine blue) and at 70% dye E102 (tartrazine yellow).
• a coloring product is thus obtained providing a green color. It is interesting to note that in the two basic colors are intimately distributed in a balanced manner in each solid element of the product, granulated or vermicelli, or lozenge or other form coming from molding.
• the procedure is as above, but with the aim of manufacturing a coloring product intended for use by a manufacturer of animal feed in the form of dry kibble.
• the starting dye is E171 dye, i.e. micronized titanium powder. It is diluted in a mixture of polyethylene glycol in the molten state and of effervescent mixture at a temperature between 50 and 70 ° C.
• the agglomerates obtained during cooling have dimensions of between 2 and 5 mm.
• the product can be dosed in the dry food mixture to reach a concentration of approximately 10% by coloring E171 itself.
• this dye is used directly without having undergone the treatment according to the invention, it is hardly known to exceed a concentration of 0.5% by weight.
• the inorganic dye of titanium dioxide E 171 is replaced by tartrazine dye E1 02, as it is used in a known manner in this kind of dry food to present there a final concentration of 0, 1% by weight.
• the two dyes are combined in the same dye product according to the invention by simultaneously introducing them for dissolution or pseudo-solution in the molten polyethylene glycol, in admixture with the constituents of the effervescent mixture. It is observed on this occasion that the mixture of dyes and their respective dosages are ensured in the manufacture of the product according to the invention and that the client no longer has any need to handle the dirty dust. It is also guaranteed to obtain the desired shade in a reproducible manner.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Polymers & Plastics (AREA)
• Food Science & Technology (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Zoology (AREA)
• Organic Chemistry (AREA)
• Animal Husbandry (AREA)
• Health & Medical Sciences (AREA)
• Nutrition Science (AREA)
• Coloring Foods And Improving Nutritive Qualities (AREA)
• Detergent Compositions (AREA)

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• 2001
  • 2001-06-22 FR FR0108575A patent/FR2826369B1/fr not_active Expired - Lifetime
• 2002
  • 2002-06-21 WO PCT/FR2002/002163 patent/WO2003000800A2/fr not_active Ceased
  • 2002-06-21 AU AU2002350306A patent/AU2002350306A1/en not_active Abandoned
  • 2002-06-21 US US10/481,575 patent/US20040216643A1/en not_active Abandoned
  • 2002-06-21 CA CA2450920A patent/CA2450920C/fr not_active Expired - Fee Related
  • 2002-06-21 EP EP02780843A patent/EP1397436A2/de not_active Withdrawn

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