Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D9/00—Crystallisation
  • B01D9/0004—Crystallisation cooling by heat exchange
  • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/37—Esters of carboxylic acids
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
  • A61Q1/14—Preparations for removing make-up
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
  • A61Q19/10—Washing or bathing preparations
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
  • A61Q5/02—Preparations for cleaning the hair
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
  • C09K23/02—Alkyl sulfonates or sulfuric acid ester salts derived from monohydric alcohols
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
  • C09K23/22—Amides or hydrazides
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
  • C09K23/42—Ethers, e.g. polyglycol ethers of alcohols or phenols

Definitions

• the present invention relates to an improved process for preparing a fluid-based, concentrated, fatty acid-based crystal ingredient as well as the use of this fluid concentrated ingredient.
• Crystals of fatty acid esters for example ethylene glycol distearate (or EthyleneGlycol DiSteArate - EGDS) crystals are commonly used in cosmetic formulations, as agents providing some pearlscence and / or as thickening agents and / or as stabilizing agents. These crystals can be formed during the preparation of the cosmetic composition, however for practical and economical reasons they are often marketed in the form of ready-to-use fluid concentrate ingredients intended to be mixed with the other ingredients of the cosmetic formulation.
• ethylene glycol distearate or EthyleneGlycol DiSteArate - EGDS
• DE 3617306 (Henkel) describes a process for the preparation of products based on a fatty acid ester in which a heated emulsion based on the fatty acid ester is cooled slowly without flowing.
• WO9503782 discloses a process for preparing products based on a fatty acid ester in which a heated emulsion based on a fatty acid ester is slowly cooled. Cooling is indicated as up to about 0.25 ° C. per minute (15 ° C. per hour).
• the document US4486334 (Lion) describes a process for the preparation of products based on a fatty acid ester in which a fatty acid ester in liquid-solubilized form is slowly cooled with a surfactant. The cooling method is not indicated. Such a method is impractical and can not be modulated because it strongly depends on the ability to form liquid crystals depending on the surfactants.
• the homogeneity and the kinetics of the cooling process are notably related to the stirring conditions in the reactor.
• the lower the stirring conditions of the medium the longer and less homogeneous the cooling.
• Conducting the entire cooling of the emulsion with stirring can be difficult without significant degradation of the optical properties of the concentrate. In this case it is necessary to practice a part of the cooling in the absence of any agitation to obtain strong pearlescence concentrates.
• This constraint induces, during the industrialization of the process, extrapolation difficulties and significantly hinders productivity.
• the industrial implementation of reactors of 10 to 25 m 3 may require from one to several days to finalize this operation. Such times show low productivity.
• the properties of the concentrates obtained industrially are generally worse than those acquired at the laboratory scale.
• the invention provides a process for preparing a fluid concentrated ingredient comprising crystals based on a fatty acid ester, comprising the following steps: step a) preparing an emulsion comprising water, a compound based on a fatty acid ester, and the surfactant (s), said emulsion being at a temperature above the melting temperature of the compound based on the fatty acid ester, step b) cooling the emulsion at a temperature below the melting temperature of the compound, so as to form the crystals, by implementing at least one cooling phase by introduction of a flow of the emulsion and flow in a cooling device allowing agitation of the flow generated by its own flow, step c) recovering downstream of the cooling device a flow of a fluid comprising the crystals and the surfactant (s), step d) optionally operating a cooling complementary to the fluid step e) optionally adding other compounds to the fluid and / or diluting the fluid and / or mixing the fluid, step f) recovering the concentrated fluid ingredient
• the invention also relates to uses of the products obtained in foaming formulations, especially in cosmetic formulations, typically by mixing with the other ingredients of these formulations.
• the invention also relates to a process for the preparation of such formulations, typically involving a preparation phase of the concentrated fluid ingredient, and then a mixing phase with the other ingredients.
• the method makes it possible to obtain at least one of the following improvements:
• the implementation of the method makes it possible to determine whether the fluid concentrated ingredients prepared at the laboratory scale by the process of the invention can likewise be prepared on an industrial scale. With the aid of the processes of the prior art it can be very long and very difficult, if not impossible, to industrialize fluid concentrated ingredients tested at the laboratory scale.
• the term fluid concentrated ingredient a composition comprising at least 5% by weight of the crystals, preferably at least 10% by weight, preferably less than 35% by weight, typically 15 to 30% by weight for example 15 to 18% or 18 to 22%, or 22 to 26%, or 26 to 30%.
• the ingredient is most often intended to be used for the preparation of cosmetic formulations such as shampoos, after shampoos or shower gels, comprising other ingredients, and more diluted in crystals.
• the term concentrated fluid ingredient is thus particularly used as opposed to finished cosmetic formulations.
• the fluid concentrate ingredient can be referred to as cold pearl concentrate.
• fatty acid ester compound is meant a compound or a composition comprising at least 75% by weight of a fatty acid, and optionally other compounds.
• FIG. 1 represents an embodiment of a cooling device that can be used, alone or in modules, for implementing step b).
• FIG. 2 represents a schematic diagram of a particular embodiment of the method, where quenching is performed, and where step d) and e) are not performed.
• FIG. 3 represents an embodiment of a cooling device using a Sulzer® Mixer Reactor (SMR®) type exchanger.
• SMR® Sulzer® Mixer Reactor
• the fatty acid ester compound is a solid compound at room temperature, preferably at a temperature of 25 ° C. It may especially be a compound whose melting point is greater than 30 ° C., preferably at 40 ° C., preferably at 50 ° C.
• the fatty acid ester on which are the crystals may in particular be a fatty acid ester with a diol or a polyol of formula (I) below:
• R is a linear or branched C 1 -C 21 , preferably C 15 -C 21 , saturated or unsaturated hydrocarbon-based group;
• A is a hydrocarbon group, optionally interrupted by one or more heteroatoms, of valence x + y,
• x is an average number between 1 and 5
• y is an average number of between 0 and 5; x + y is an average number of between 1 and 10, preferably between 2 and 5; In the present application, an average number can designate an integer or a decimal number. In the present application, the expression "between X and Y" includes the terminals X and Y.
• Group A is a group whose compound of formula A - (- OH) x + y is a diol or a polyol. It may especially be a diol such as ethylene glycol, or a polyol such as glycerol. advantageously:
• Group A may in particular present the following formula:
• z identical or different, is an integer from 1 to 10,
• - OE is an optional ethylene oxide group
• n is an average number between 0 and 100, preferably 0 to 10, and
• OP is an optional propylene oxide group
• m is an average number of between 0 and 100, preferably 0 to 10.
• the compound of formula A - (- OH) 2 may be a product of (poly) ethoxylation and / or (poly) propoxylation, or of ethylene glycol condensation and / or propylene glycol.
• the group A does not include EO and / or PO, and it is alkylene CRCI 0, preferably C 2 -C 4.
• the group A can in particular be a methylene, ethylene, propylene or butylene group or a mixture of these groups.
• the R group is a hydrocarbon group, for example an alkyl group, saturated or unsaturated, linear or branched -C 3 -C 2I, preferably C 5 -C 2I. It is an alkyl group corresponding to a fatty acid of formula R-COOH, Ci 4 -C 22 , preferably Ci 6 -C 22 . These fatty acids and alkyl groups are known. These are generally derived from vegetable oils. They can be present in mixtures. In the case of mixtures, the definition of all the groups, irrespective of the number of carbon atoms, if the group (or the corresponding acid) predominates in weight (relative majority, preferably absolute preferably at least 75%) corresponds to the definition.
• the group R may in particular correspond to C1 4 or Ci 6 or Ci 8 or C 22 fatty acid, such as myristic, palmitic, stearic, oleic, erucic or behenic acids.
• R-COO- corresponds to a fatty acid Ci 8, preferably stearic acid. It is particularly advantageous to use a compound based on ethylene glycol distearate (or "Ethylene Glycol Di-Stearate" - EGDS).
• compound “based on ethylene glycol distearate” is meant a compound or a composition comprising at least 75% by weight of ethylene glycol distearate, and optionally other compounds, especially ethylene glycol monostearate (EGMS). .
• EGMS ethylene glycol monostearate
• distearate of ethylene glycol or the acronym EGDS will denote a compound based on ethylene glycol distearate.
• the fatty acid ester comprises at least 80% by weight of ethylene glycol distearate, and optionally ethylene glycol monostearate. It can include:
• ethylene glycol monostearate from 1% to 20% by weight, preferably from 10% to 20%, preferably approximately 15%, of ethylene glycol monostearate.
• the method of the invention uses at least one surfactant.
• the surfactant (s) makes it possible in particular to form the emulsion.
• a surfactant system we implement a single surfactant or several surfactants.
• the surfactant system may in particular comprise a nonionic surfactant and / or anionic surfactant. It is not excluded that it comprises at least one amphoteric surfactant such as betaines (for example alkyldimethylbetins or alkyldimethylamidoalkylbetals) or imidazoline derivatives (for example alkylamphoacetates or alkylamphodiacetates).
• amphoteric surfactant such as betaines (for example alkyldimethylbetins or alkyldimethylamidoalkylbetals) or imidazoline derivatives (for example alkylamphoacetates or alkylamphodiacetates).
• betaines for example alkyldimethylbetins or alkyldimethylamidoalkylbetals
• imidazoline derivatives for example alkylamphoacetates or alkylamphodiacetates.
• the surfactant (s) anionic (s) and / or nonionic (s), it may for example be an ethoxylated fatty alcohol optionally sulfated, such as an ethoxylated fatty alcohol (nonionic surfactant) ) or a sulphated ethoxylated fatty alcohol (anionic surfactant).
• the surfactant is an anionic surfactant, for example a sulphated ethoxylated fatty alcohol, it is generally in the form of a salt, for example a sodium or ammonium salt.
• the surfactant system comprises:
• nonionic surfactant preferably an ethoxylated fatty alcohol
• surfactant preferably selected from anionic surfactants, amphoteric surfactants, nonionic surfactants different from ethoxylated fatty alcohol, and mixtures thereof.
• the surfactant system comprises:
• an anionic surfactant preferably a sulphated ethoxylated fatty alcohol
• Another surfactant preferably selected from nonionic surfactants, amphoteric surfactants, anionic surfactants different from sulfated ethoxylated fatty alcohol, and mixtures thereof.
• ethoxylated fatty alcohols nonionic surfactants
• the fatty alcohols are generally mixtures derived from vegetable products or from petroleum cuts.
• the number of carbon atoms can be an average number or the carbon number of the predominant species.
• These fatty alcohols are ethoxylated.
• the average number by number of ethoxy units may be from 1 to 25, preferably from 5 to 9.5.
• Particularly useful fatty alcohols are ethoxylated fatty alcohols -C 0 -C 4, ethoxylated with an average number as the number of ethoxy units is 5 to 9.5, preferably 5 to 9, for example 7 or 9.
• the anionic surfactant may for example be chosen from saturated or unsaturated, branched or linear alcohols, Ci 0 -Ci 4 ethoxylated and sulfated. It may for example be a tridecyl alcohol preferably ethoxylated branched 2 to 10 times, for example ethoxylated 3 times, and sulfated.
• Rhodapex EST 30 sold by Rhodia (INCI: sodium trideceth-3 sulfate).
• amphoteric surfactant may especially be chosen from alkylamidopropyl betaines, such as cocamidopropyl betaine, and / or imidazoline derivatives, such as alkylamphoacetates or alkylamphodiacetates, in particular lauroamphoacetate or diacetate or cocoamphoacetate or diacetate.
• the fluid concentrated ingredient comprises:
• the amounts of fatty acid ester and surfactant (s) used may be adjusted accordingly during the implementation of the method. It is not excluded to operate, at the end of the process or after, dilutions by adding water or other ingredients.
• the fluidized concentrated ingredient may in particular comprise additives such as preservatives (generally in minor amounts, for example of the order of 0.1% by weight), buffers, stabilizing agents, agents for modifying optical properties.
• the fluid concentrated ingredient may have a viscosity of 10 to 10,000 Pa.s, for example 100 or 500 to 5000 Pa.s at 20 ° C., at a shear of 0.1 s -1 , measured using a plane-plane flow rheometer such as the Rheometrics® ARES equipped with the 50 mm module.
• step a) an emulsion is prepared comprising water, a compound based on a fatty acid ester, and surfactant (s), said emulsion being at a temperature above the temperature melting compound based on the fatty acid ester.
• Step a) may be carried out in known manner by any method for forming an emulsion at a temperature above the melting temperature of the fatty acid ester compound. In particular, it is possible to operate by melting the fatty acid ester and by emulsification in the presence of the surfactant system, subsequently or simultaneously.
• step a) comprises the following steps: a1) preparing a dispersion comprising water, solid particles based on the fatty acid ester, and surfactant (s), a2 ) heating the dispersion so as to liquefy the fatty acid ester-based particles.
• Stage a) may in particular be carried out batchwise, semi-continuously or continuously, preferably in a tank, for example a stirred tank (11).
• the temperature of the emulsion before the cooling step b) is typically greater than or equal to 1 ° C more, preferably at 5 ° C more, preferably at 10 0 C more, than the melting temperature of the fatty acid ester.
• the process is preferably carried out at a temperature greater than or equal to 55 ° C., preferably greater than or equal to 60 ° C., preferably 55 ° C. to 70 ° C., preferably 60 ° C. at 70 0 C or 65 ° C.
• step b) the emulsion is cooled to a temperature below the melting temperature of the compound to form the crystals.
• This step comprises a cooling phase by introduction of a flow of the emulsion (1) and flow in a cooling device (2) allowing agitation of the flow generated by its own flow. All or part of the cooling carried out during step b) can be performed using the cooling device. It is noted that part of the cooling can be implemented by a quenching operation, upstream of the cooling device, in the cooling device, or even downstream. Step b) may include in particular: - optionally a quenching operation, upstream of the cooling device or in the cooling device, where a quenching fluid is mixed with the flow, and / or - optionally an optional seeding operation wherein a seeding fluid comprising crystals based on a fatty acid ester compound is mixed with the stream. Details of quenching and / or seeding operations are given below.
• step b) a flow of material flows into the flow device and this flow is cooled.
• the temperature at the point of introduction of the emulsion is therefore greater than the temperature at the point of exit.
• the flow of material is transformed from an emulsion to a fluid comprising crystals at the outlet of the flow device.
• Step b) is typically operated continuously.
• the cooling carried out in step b) is preferably at least 5 ° C., preferably at least 10 ° C.
• the cooling phase carried out in the flow-through cooling device is preferably at least 5 ° C, preferably at least 10 ° C.
• the flow device typically has a flow zone (3) delimited by so-called confinement walls (4). These delimit the space where the flow flows.
• the flow zone may typically be the inside of a tubular device whose cross-section may be of varied shape, for example round, square, rectangular, ovoid.
• the tube of the tubular device may constitute all of the confinement walls, or part of the confinement walls.
• step b) the flow that flows undergoes agitation generated by the flow itself.
• Simple flow can provide agitation.
• agitation is provided by means of obstacles (5) to the flow. These obstacles are typically provided within the flow zone. These obstacles are preferably static. However, it is not excluded to provide additional agitation with mobile devices such as mobile agitators.
• the obstacles represent a volume of at least 1%, for example from 1 to 5% or from 5 to 10%, or from 10 to 15%, or from 15 to 20%, or from 20 to 25%, or 25 to 30%, or 30 to 40%, or 40 to 50%, or 50 to 75%, of the volume of the flow zone.
• Static or non-static obstacles may in particular be geometric inserts of various shapes.
• the obstacles may also consist of a set of separators and / or flow vein collectors. Cooling inserts within the flow zone can also be used as barriers.
• step b) can be carried out by any appropriate means. Such means are known to those skilled in the art. In particular, it is possible to use a cooling fluid. Such cooling operations and suitable devices are known to those skilled in the art. In particular, tubular exchangers, multitubular exchangers, spiral exchangers, plate exchangers, Sulzer® Mixer Reactor (SMR®) exchangers can be used.
• SMR® Sulzer® Mixer Reactor
• the cooling of step b) may for example be provided by a cooling fluid (6) circulating in a cooling circuit (7).
• the cooling circuit is typically defined by walls, said cooling walls (8), at least a portion of which is in contact with the flow. It is possible to refer to the wall portions in contact with the flow as delimiting a cooling zone. It is noted that the confinement walls and the cooling walls can, on at least a part, constitute a common wall separating the flow zone from the cooling circuit, that is to say separating the flow from the cooling fluid. Note that it may be walls or parts of walls of the same room, or of several parts in contact (for example glued, welded or nested) on the walls or parts of walls. In the embodiment shown in Figure 1 the containment walls (4) and cooling (8) are combined.
• the cooling circuit is placed inside the flow zone, the circuit constituting obstacles to the flow.
• a particular variant of this embodiment is illustrated with reference to FIG. 3.
• SMR® Sulzer® Mixer Reactor
• the cooling circuit is placed outside the flow zone.
• the flow zone may for example consist of at least one tubular duct constituting the confinement walls, provided inside a static mixer, at least a portion of the confinement walls constituting a common wall with at least a part of the cooling circuit.
• the cooling device may for example be a double jacket tubular exchanger, where the cooling circuit is a tubular circuit inside which is disposed an internal tubular duct inside which flow flows.
• a succession of cooling circuits is implemented in which a succession of cooling fluids with equal or variable introduction temperatures, for example increasing or decreasing, flows.
• a succession of cooling fluids with equal or variable introduction temperatures for example increasing or decreasing
• the cooling device of step b) consists of a succession of modules (9) constituting cooling devices as described above.
• Figure 2 illustrates such a particular embodiment.
• the module of (9) may be a device as illustrated in FIG.
• quenching is carried out by mixing a cold quenching fluid (10) at a temperature that is less than or equal to the temperature of the flow at the point where the mixture is blended. preferably less than or equal to the melting point of the fatty acid ester compound.
• This mixing can be carried out upstream of the flow device and / or the flow zone and / or the zone in contact with the cooling circuit, or at a point of the flow situated on the first quarter, of preferably the first eighth, preferably the first sixteenth, of the flow device and / or the flow zone in the cooling device, for example the cooling zone.
• the quenching fluid may especially be at a temperature of less than or equal to 25 ° C.
• the quenching fluid may be pure water or comprising additives.
• the quenching fluid may comprise, as primer or seed, crystals based on the fatty acid ester compound.
• the quenching fluid may be a part of the fluid recovered after steps c), d), or e). Priming or seeding can facilitate the appearance of crystals, and / or promote the production of certain crystalline forms, and thus facilitate the mastery of the optical properties obtained.
• the implementation of a quenching fluid is illustrated in FIG.
• seeding can be carried out by mixing the flow of a seeding fluid at a temperature not lower than or equal to the melting temperature of the fatty acid ester compound. This mixing can be carried out upstream of the flow device and / or the flow zone and / or the zone in contact with the cooling circuit, or at a point of the flow situated on the first quarter, of preferably the first eighth, preferably the first sixteenth, of the flow device and / or the flow zone in the cooling device, for example the cooling zone.
• the seeding fluid comprises, as primer or seed, crystals based on the fatty acid ester compound.
• the seeding fluid may be a part of the fluid recovered after steps c), d), or e).
• Priming or seeding can facilitate the appearance of crystals, and / or promote the production of certain crystalline forms, and thus facilitate the mastery of the optical properties obtained.
• a fluid comprising crystals is mixed, it is a so-called quench fluid fluid or a so-called seeding fluid fluid depending on the temperature.
• the cooling device may in particular be equipped with probes for measuring the temperature and / or the pressure of the flow and / or the temperature of the coolant. Such probes can in particular make it possible to control the process.
• step b) does not cause clogging and shielding phenomena in the flow device, especially in the presence of static mixers.
• fatty acid ester compound of surfactant (s) as follows: a quantity of fatty acid ester compound such as the product recovered in step c) comprises at least 5% by weight, preferably at least 10%, preferably at least 15%, of the fatty acid ester. an amount of surfactant (s) such as the product recovered in stage c) comprises at least 2.5% by weight, preferably 5% by weight, preferably at least 10%; surfactant (s).
• step a) is carried out continuously, discontinuously or sequentially, and
• step b) is implemented continuously.
• a flow of a fluid (13) comprising the crystals and the surfactant (s) is recovered downstream of the cooling device. It can be a flow at room temperature, or a still hot flow.
• a step d) of complementary cooling of the fluid can be implemented in a device with continuous flow, or in a device without flow, statically, discontinuously or semi-continuously.
• Step d) may in particular be carried out in a tank, if necessary agitated, allowing to cool to room temperature, or by controlling the cooling.
• the tank can be cooled with or without cooling means such as jacketed cooling circuits and / or internal coils.
• the additional cooling of step d), after formation of the crystals is less critical for the properties of the concentrated fluid ingredient to be prepared. It can be implemented without affecting productivity and / or properties.
• the fluid comprising the crystals and the surfactant (s) recovered in step c) and / or in step d) may constitute the desired fluid concentrate ingredient.
• the composition of the fluid can be adjusted to obtain the desired fluid concentrate ingredient.
• an optional step e) where other compounds are added to the fluid and / or the fluid is diluted and / or the fluid is mixed.
• step e) it is thus possible to adapt the composition of the fluid concentrate ingredient to the final formulation for which it is intended.
• Step e) can in particular be carried out in a tank, preferably by stirring.
• step e) it is possible in particular to add water or solvents, preservatives, pH control agents, optical property modifiers, suspension stabilizers, other surfactants (or adjust the concentration of the surfactants already present), dispersants.
• steps d) and e) can be implemented simultaneously or subsequently, in order d) then e) or e) then d). It is specified that in the case where steps d) and e) are not performed, steps c) and f) are combined. In steps c) and / or f), for example, the flow and / or the concentrate can be recovered in a vessel and / or in a container (14) allowing transport.
• the method of the invention makes it possible in particular to prepare fluid concentrated ingredients having excellent and stable pearlscence and opacity properties.
• step b) made it possible to conclude that the cooling of the emulsion could not be limited by the heat exchange capacities but could be controlled but by the kinetics of crystallization. In particular, this makes it easier to determine whether the fluid concentrated ingredients prepared at the laboratory scale are industrially feasible, and therefore whether their properties can be preserved during industrial scale-up.
• the fluid concentrated ingredients obtained by the process of the invention can be used in formulations comprising in addition to other ingredients. It is preferably the formulation of consumer products. This may include cosmetic formulations or formulation or home care. These formulations can in particular be foaming formulations. It may for example be products for cleaning dishes by hand or machine. They may also be products for cleaning hard surfaces, for example for cleaning floors or toilets. It may also be formulations for cleaning, care or shaping of the hair, for example in shampoos or hair conditioners, or in cleaning or skin care formulations, for example in gels. shower, hygiene products, makeup removers.
• cosmetic formulations or formulation or home care These formulations can in particular be foaming formulations. It may for example be products for cleaning dishes by hand or machine. They may also be products for cleaning hard surfaces, for example for cleaning floors or toilets. It may also be formulations for cleaning, care or shaping of the hair, for example in shampoos or hair conditioners, or in cleaning or skin care formulations, for example in gels. shower, hygiene products, makeup removers.
• the crystals may especially be used as an agent for modifying the visual perception of the formulation (glossy and / or opaque and / or pearlescent aspect in particular), and / or as an agent for modifying the appearance of the hair (glossy appearance and / or opaque and / or pearlescent in particular), and / or as an agent promoting the suspension (stabilizer for example) of solid or liquid particles (emulsions). It may be in particular a use as a modulating agent brightness and opacity, providing preferably glossy and opaque pearlescent important with reflections of the several colors.
• the amount of fluid concentrated ingredient used may be such that the amount of crystals included in the formulation is less than 5% by weight, typically 1 to 4% by weight.
• the formulations may comprise all the ingredients generally used in the fields of application under consideration.
• the formulations may in particular comprise surfactants.
• cosmetically acceptable vectors in particular aqueous, alcoholic or hydroxyalcoholic vectors,
• nonionic, anionic, cationic, amphoteric surfactants including zwitterionic surfactants
• nonionic, anionic, cationic, amphoteric surfactants including zwitterionic surfactants
• amphoteric surfactants including zwitterionic surfactants
• mixtures thereof in particular those mentioned as being able to be present in the fluid concentrated ingredient, active agents, in solubilized form or in the form of solid or liquid particles, for example anti-dandruff particles, mineral or organic UV filters
• silicones can in particular be in solubilized or dispersed form, in particular dimethicones, amodimethicones, dimethiconols, cationic silicones, silicones comprising polyethylene glycol blocks, in the form of oils, or of emulsion of average size greater or less than at 2 ⁇ m, or in the form of microemulsions smaller than 0.15 ⁇ m, or even in the form of solubilized.
• the emulsification can be carried out in situ or beforehand.
• the viscosity of the silicones may be, for example, less than 50,000 cP, or between 50,000 and 200,000 cP, or greater than 200,000 cP.
• conditioning and / or stabilizing polymers and / or suspending and / or viscosizing agents of natural or synthetic origin in particular:
• cationic or amphoteric polymers such as cationic guars, cationic polysaccharides, for example PQ-10, synthetic cationic polymers such as PQ-7, synthetic amphoteric polymers such as
• thickening and / or stabilizing agents derived from natural polymers such as the optionally partially depolymerized non-grafted guar, hydroxypropyl guars; Xanthan gum,
• - fatty acid esters -C 0 -C 30 preferably C 16 -C 22 and of polyols or monohydric alcohols or ethers of fatty alcohols -C 0 -C 30 preferably a C 6 -C 22 different EGDS, for example distearyl ether, polyethoxylated and / or polypropoxylated stearates or distearates, for example PEG-3 distearates, PEG / PPG distearates, PEG-200 distearates, PEG-150 distearates, PEG-100 stearates
• Cosmetically acceptable vector Any cosmetically acceptable vector for formulating the ampholyte polymer and obtaining the desired cosmetic composition form, for the intended use, may be used. Different cosmetically acceptable vectors for different types of formulations are known to those skilled in the art.
• aqueous vectors comprising water
• alcoholic vectors comprising an alcohol, for example ethanol, isopropanol, ethylene glycol or polyethylene.
• glycol for example ethanol, isopropanol, ethylene glycol or polyethylene glycol
• hydro-alcoholic carriers comprising a mixture of water and an alcohol, for example ethanol, isopropanol, ethylene glycol or polyethylene glycol.
• Some oils, volatile or not, can also be used.
• fluid silicones such as cyclopentasiloxane, for example Mirasil CM5 marketed by Rhodia, are mentioned.
• aqueous vectors are generally used for shampoos or shower gels.
• a propylene glycol vector may be used in the form of creams.
• a cyclomethicone vector can be used for make-up compositions, for example for foundations.
• the formulation may comprise at least one surfactant (iv). It can be a mixture of different surfactants.
• the surfactants may be anionic, cationic, nonionic, amphoteric surfactants or mixtures or combinations.
• the surfactants included in the composition preferably comprise at least one anionic or cationic surfactant.
• the surfactants may also comprise amphoteric surfactants (true or zwitterionic amphoters), neutral surfactants (nonionic surfactants).
• Formulations comprising at least one anionic surfactant and at least one amphoteric surfactant are particularly advantageous, especially for reasons of softness.
• the total content of surfactants in the composition is generally between 0 and 30% by weight.
• the surfactant is preferably absent or present in an amount of less than 5% by weight, and may be preferably a cationic surfactant.
• the surfactant content is advantageously between 10 and 20% by weight.
• Such formulations may comprise salts, for example sodium or ammonium chloride, advantageously in a content of less than 3% by weight.
• the surfactant content is advantageously between 5 and 15% by weight.
• Such formulations also preferably comprise at least 2% by weight of salts, for example sodium or ammonium chloride.
• the surfactant content may be less than 5% by weight.
• the proportion by weight of anionic surfactants relative to all the surfactants is preferably greater than 50%, preferably greater than 70%.
• the anionic surfactants may be chosen from the following surfactants: alkyl ester sulfonates, for example of formula R-CH (SO 3 M) -CH 2 COOR ', or alkyl ester sulfates, for example of formula R-CH (OSO 3 M) - CH 2 COOR ', where R represents a C 8 -C 2 O alkyl radical, preferably C 10 -C 16 alkyl radical, R' a C 1 -C 6 alkyl radical, preferably a dC 3 alkyl radical, and M an alkaline earth metal cation, for example sodium, or the ammonium cation.
• alkyl ester sulfonates for example of formula R-CH (SO 3 M) -CH 2 COOR '
• alkyl ester sulfates for example of formula R-CH (OSO 3 M) - CH 2 COOR '
• R represents a C 8 -C 2 O alkyl radical, preferably C 10
• methyl ester sulfonates whose radical R is C 1 -C 6 ; alkylbenzenesulfonates, more particularly C 9 -C 20 , primary or secondary alkylsulfonates, especially C 8 -C 22 , alkylglycerol sulfonates; alkyl sulphates, for example of formula ROSO 3 M, where R represents a C 1 -C 24 , preferably C 1 -C 20 , alkyl or hydroxyalkyl radical; M a cation of the same definition as above; alkyl ether sulfates, for example of the formula RO (OA) n SO 3 M, where R represents a C 1 -C 24 , preferably C 1 -C 20 , alkyl or hydroxyalkyl radical; OA representing an ethoxylated and / or propoxylated group; M representing a cation of the same definition as above, n generally ranging from 1 to 4,
• the nonionic surfactants may be chosen from the following surfactants: alkoxylated fatty alcohols; for example laureth-2, laureth-4, laureth-7, oleth-20 - alkoxylated triglycerides alkoxylated fatty acids alkoxylated sorbitan esters alkoxylated fatty amines alkoxylated di (1-phenylethyl) phenols - tri (phenyl) The alkoxylated alkyl phenols; the products resulting from the condensation of ethylene oxide with a hydrophobic compound resulting from the condensation of propylene oxide with propylene glycol, such as Pluronic sold by BASF; the products resulting from the condensation of ethylene oxide with the compound resulting from the condensation of propylene oxide with ethylenediamine, such as Tetronic marketed by BASF; alkylpolyglycosides such as those described in US 4565647 or alkylglucosides; fatty acid amides, for
• amphoteric surfactants may be chosen from the following surfactants: betaines in general, in particular carboxybetaines from, for example, lauryl betaine (Mirataine BB from Rhodia) or octylbetaine or cocobetaine (Mirataine BB-FLA from Rhodia); amidoalkyl betaines, such as cocamidopropyl betaine (CAPB) (Mirataine BDJ from Rhodia or Mirataine BET C-30 from Rhodia);
• betaines in general, in particular carboxybetaines from, for example, lauryl betaine (Mirataine BB from Rhodia) or octylbetaine or cocobetaine (Mirataine BB-FLA from Rhodia); amidoalkyl betaines, such as cocamidopropyl betaine (CAPB) (Mirataine BDJ from Rhodia or Mirataine BET C-30 from Rhodia);
• CAPB cocamidopropyl betaine
• sulfobetaines or sultaines such as cocamidopropyl hydroxy sultaine (Mirataine CBS from Rhodia);
• alkylamphoacetates and alkylamphodiacetates such as for example comprising a coco and lauryl chain (Miranol C2M Conc NP, C32 and L32, in particular, from Rhodia);
• alkylamphopropionates or alkylamphodipropionates (Miranol C2M SF); alkyl amphohydroxypropyl sultaines (Miranol CS),
• alkyl amine oxides for example lauramine oxide (INCI).
• the cationic surfactants may be chosen from salts of primary, secondary or tertiary fatty amines, optionally polyethoxylated, quaternary ammonium salts such as chlorides or bromides of tetraalkylammonium, alkylamidoalkylammonium, trialkylbenzylammonium, trialkylhydroxyalkylammonium, or alkylpyridinium, imidazoline derivatives, cationic amine oxides.
• An example of a cationic surfactant is cetrimonium chloride or bromide (INCI).
• Sodium formulations for shampoos typically comprising 12 to 16% by weight of sodium alkylethersulphate (for example sodium laurylethersulphate “SLES”) or of a mixture of sodium alkylethersulfate and sodium alkylsulphate (for example sodium lauryl sulphate “SLS”), 1 to 3% of an amphoteric surfactant (for example cocoamidopropylbetaine "CAPB”), 0.5 to 2% of a salt (for example sodium chloride).
• sodium alkylethersulphate for example sodium laurylethersulphate "SLES”
• SLS sodium lauryl sulphate
• an amphoteric surfactant for example cocoamidopropylbetaine "CAPB”
• CAPB cocoamidopropylbetaine
• Ammonium formulations for shampoos typically comprising 12 to 16% by weight of ammonium alkyl ether sulphate (for example ammonium lauryl ether sulphate “ALES”) or a mixture of ammonium alkyl ether sulphate and alkyl sulphate.
• ammonium for example ammonium lauryl sulphate “ALS”
• a surfactant amphoteric eg cocoamidopropylbetaine "CAPB”
• a salt eg ammonium chloride
• the “sodium" formulations for gel-shower typically comprising 6 to 10% by weight of sodium alkylethersulfate (for example sodium laurylethersulfate “SLES”) or of a mixture of sodium alkylethersulfate and sodium alkylsulphate (for example sodium lauryl sulphate “SLS”), 1 to 3% of an amphoteric surfactant (for example cocoamidopropylbetaine "CAPB”), 2 to 4% of a salt (for example sodium chloride).
• sodium alkylethersulfate for example sodium laurylethersulfate "SLES”
• SLS sodium lauryl sulphate
• an amphoteric surfactant for example cocoamidopropylbetaine "CAPB”
• CAPB cocoamidopropylbetaine
• the "sodium" formulations for gel-shower typically comprising 6 to 10% by weight of ammonium alkylethersulfate (for example ammonium laurylethersulphate)
• ALES ammonium alkylethersulfate and ammonium alkylsulphate
• ALS ammonium laurylsulphate
• an amphoteric surfactant for example cocoamidopropylbetaine "CAPB”
• a salt eg ammonium chloride
• An emulsion having the following composition (quantities by weight of material as is) is prepared in a stirred tank: - EGDS * 23.50%
• the temperature of the emulsion is 65 ° C.
• a piston pump the emulsion is withdrawn from the tank and introduced at 65 ° C in the cooling device described below.
• the device is formed of 6 series of cooling modules of tubular conduits, each consisting of a tubular conduit wrapped by a countercurrent cooling circuit, and provided with a static mixer.
• Figure 1 shows a diagram of a module. The cooling fluid flows from right to left in FIG. 1. The emulsion flows from left to right in FIG. 1. The characteristics of each module are given: - metal tube 15 mm internal diameter.
• the operating conditions of the cooling are as follows:
• a fluid concentrated ingredient having crystals based on EGDS having optical properties (pearlscence) similar to those obtained using a process involving discontinuous crystallization in a batch-type batch reactor is obtained.
• agitated cooled under much lower productivity conditions for example expressed by weight of cooled material per hour and optionally by volume occupied).

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