EP1183100A1 - Mineral-salt based substantially or totally hydrosoluble composition, formulation containing said composition and production thereof - Google Patents

Mineral-salt based substantially or totally hydrosoluble composition, formulation containing said composition and production thereof

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Publication number
EP1183100A1
EP1183100A1 EP00917117A EP00917117A EP1183100A1 EP 1183100 A1 EP1183100 A1 EP 1183100A1 EP 00917117 A EP00917117 A EP 00917117A EP 00917117 A EP00917117 A EP 00917117A EP 1183100 A1 EP1183100 A1 EP 1183100A1
Authority
EP
European Patent Office
Prior art keywords
composition
water
composition according
optionally
mineral salt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00917117A
Other languages
German (de)
French (fr)
Inventor
Jean-Pierre Hecaen
Laurent Taisne
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhodia Chimie SAS
Original Assignee
Rhodia Chimie SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rhodia Chimie SAS filed Critical Rhodia Chimie SAS
Publication of EP1183100A1 publication Critical patent/EP1183100A1/en
Withdrawn legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/34—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/28—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using special binding agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0281—Sulfates of compounds other than those provided for in B01J20/045
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3028—Granulating, agglomerating or aggregating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/14—Fillers; Abrasives ; Abrasive compositions; Suspending or absorbing agents not provided for in one single group of C11D3/12; Specific features concerning abrasives, e.g. granulometry or mixtures
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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    • C11D3/16—Organic compounds
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials

Definitions

  • the subject of the present invention is a composition in the form of solid particles, substantially or completely water-soluble, comprising a mineral salt crystallizing with at least one molecule of water, a binder.
  • the composition can be obtained by a drying operation at least partially eliminating the water of crystallization of said salt.
  • the grain is obtained by atomization of a mixture comprising in particular a salt of the silicate, phosphate type, and comprising, where appropriate, other additives such as anti-redeposition agents.
  • the active ingredient optionally also additive, is then sprayed onto the grains obtained.
  • the object of the present invention is therefore to provide a composition which can serve as a matrix for an active material intended to be absorbed therein, a composition which is totally or substantially water-soluble, very absorbent and not pulverulent.
  • a first object of the invention consists of a composition, in the form of solid particles, substantially or completely water-soluble, the absorption capacity of at least one active material of which can reach 50% by weight, corresponding to the ratio of weight of the active ingredient at the sum of the composition and the active ingredient; said composition being capable of being obtained from at least one mineral salt crystallizing with at least one molecule of water, from at least one organic polymeric binder whose content is less than 30% by weight of the composition, optionally at least one surfactant, optionally at least one filler, said composition being capable of being obtained by drying eliminating at least part of the water of crystallization.
  • a second subject of the invention relates to a process for the preparation of said composition in which at least partially or completely, at least the water of crystallization is removed, present in a mixture comprising at least one aforementioned mineral salt, at least one organic binder polymer, optionally at least one surfactant, optionally at least one filler, and water which is at least in the form of water of crystallization.
  • Another subject of the invention relates to a formulation comprising at least one active material absorbed on the composition according to the invention.
  • a final object of the invention relates to the preparation of said formulation; process in which a spraying or impregnation of the active material is carried out, in the form of a liquid, on the composition according to the invention.
  • the composition according to the invention has the advantage of having a very high absorption capacity. Indeed, it is possible to absorb on the composition an amount of active material which represents the weight of the composition.
  • the composition according to the invention has an absorption which can be as high as 50% (ratio by weight of the active material to the sum of the composition and the active material).
  • the absorption capacity is measured relative to Rhodasurf ID 79, which is a nonionic surfactant (isodecyl alcohol comprising 7 ethylene oxide units - sold by Rhodia Chimie). The test consists in bringing the composition into contact with the surfactant, at room temperature, gradually and with stirring, until the mixture takes on a tacky appearance (the solid mixture no longer flows fluidly - not free-flowing ). The amount of surfactant added is then evaluated.
  • the composition according to the invention Because of its pH, the composition according to the invention has the advantage of being compatible with many fields of use as varied as detergency, the food sector, the pharmaceutical industry, the agrochemical industry. Furthermore, the composition according to the invention consists of non-pulverulent porous particles, the size of which is sufficient so as not to pose handling problems.
  • the attrition resistance of the particles of the composition is improved, which has obvious advantages for the storage and handling of the composition.
  • composition according to the invention can be used to obtain solid formulations while the active material is liquid, molten or dissolved.
  • composition according to the invention has the advantage of being able to mix, in the same packaging, substances which would have been incompatible in a liquid mixture (if the substances are chemically reactive with one another, for example).
  • composition according to the invention can be adapted according to the active materials for which it will serve as a support.
  • the composition according to the invention can be advantageously used for active materials sensitive to pH. It should be noted as an additional advantageous characteristic of the composition according to the invention that it contributes to facilitating the use of the subsequent formulation which contains it. In fact, the composition according to the invention gives said formulation, more or less rapid and above all, adjustable dissolution properties.
  • the hardness of the granule (resistance to attrition), its absorption capacity, its pH, can also, and this represents advantageous characteristics of the composition of the invention, be adjusted according to the subsequent uses of the formulations which comprise it. .
  • the composition according to the invention comprises an inorganic salt crystallizing with at least one molecule of water.
  • the mineral salt is chosen from alkali metal phosphates, alkali metal carbonate, alkali metal or aluminum sulfate, alkali metal borate, aluminum salts, magnesium chloride, or mixtures thereof .
  • the alkali metal phosphates the pyrophosphate, tripolyphosphate, mono-, di- or tri-sodium phosphate, hexametaphosphate, or mixtures thereof, are suitable for implementing the invention.
  • the composition according to the invention comprises as mineral salt at least one salt chosen from phosphates, and in particular those mentioned, as well as the alkali metal carbonates, and more particularly sodium.
  • the mineral salts used for the preparation of the composition according to the invention do not comprise tripolyphosphate alone.
  • the salts used do not comprise tripolyphosphate either alone or combined with one or more other salts.
  • the amount of mineral salt represents 50 to less than 100% by weight of the composition.
  • the amount of mineral salt is between 70 and less than 100% by weight relative to the same reference.
  • the amount of mineral salt is between 85 and less than 100% by weight relative to the same reference.
  • the composition according to the invention also comprises at least one organic polymeric binder.
  • binders chosen from monosaccharides and oligosaccharides.
  • natural polymers of the type of polysaccharides of animal, plant, bacterial origin synthetic polymers of the type of polyalkyleneglycols, polyvinyl alcohol, polymers of (meth) acrylic acid or copolymer of (meth) acrylic acid and isobutylene or diisobutylene, polyacrylic acids and their salts, anhydride (or acid) copolymers maleique and isobutylene or diisobutylene, and their salts, and mixtures thereof.
  • Lactose and sucrose alone or as a mixture, represent possible examples of binders chosen from monosaccharides and oligosaccharides.
  • non-limiting examples that may be mentioned are xanthan gum, guar and derivatives (such as hydroxypropyl guar for example), polydextroses, or combinations thereof.
  • polyethylene glycols, polypropylene glycols, polybutylene glycols, polyethylene- and polypropylene glycol copolymers, polyvinyl alcohol, acid polymers are especially suitable, alone or as a mixture.
  • acrylic acid polymers such as Geropon® HB, as well as copolymers of maleic anhydride (or acid) and diisobutylene.
  • copolymers can be in the acid form or in the form of an alkali metal or ammonium salt of type N (R) 4 + , with R, identical or different, representing hydrogen atoms, or hydrocarbon radicals in C1-C4.
  • R alkali metal or ammonium salt
  • the copolymer is in the form of the sodium salt.
  • the amount of binding agent is more particularly between 0 excluded and 30% by weight of the composition according to the invention.
  • the amount of binder is between 0 excluded and 15% by weight relative to the same reference.
  • the content of binder is between 0.5 and 15% by weight relative to the composition.
  • the composition according to the invention only comprises the mineral salt and the polymeric binder, the respective contents of these compounds are such that the whole represents 100% by weight.
  • the weight ratio between the mineral salt and the binder is between 99.5 / 0.5 and 60/40. More particularly, said weight ratio is between 99.5 / 05 and 70/30, preferably between 99.5 / 0.5 and 85/15.
  • composition according to the invention can likewise comprise, if necessary, at least one surfactant.
  • the surfactant when it is present, has two roles, that of optimizing the wetting of the mineral salt and of the binder, and that of optimizing the dispersion of the active material during its use .
  • anionic, nonionic, cationic, zwitterionic or amphoteric surfactants can be used.
  • anionic surfactants that may be mentioned by way of example: ° Polymers derived from lignin, such as sodium or calcium lignosulfonates; ° the alkyl esters sulfonates of formula R-CH (S ⁇ 3M) -COOR ', where R represents an alkyl radical in C-8-C20, preferably in C10-C-16, R "an alkyl radical in Ci-C ⁇ , preferably in C1-C3 and M an alkali cation (sodium, potassium, lithium), substituted or unsubstituted ammonium (methyl-, dimethyl-, trimethyl-, tetramethylammonium, dimethylpiperidinium ...) or derived from an alkanolamine (monoethanolamine, diethanolamine, triethanol
  • methyl ester sulfonates the radical R of which is C14-C16; primary or secondary C8-C20 alkylsulfonates; alkylaryl sulfonates such as sodium isopropyl naphthalene sulfonate, sold under the name ® Supragil WP; C9-C20 alkylbenzenesulfonates; condensed sodium methylnaphthalene sulfonate such as Supragil MNS90®, paraffin sulfonates.
  • alkyl glycoside sulfates such as mono-, di- or tri-tristyryl polyoxyalkylene phenols
  • alkylamides sulfates of formula RCONHROSO3M where R represents an alkyl radical in C-2-C22, preferably in C6-C20, R 'an alkyl radical in C2-C3, M representing a hydrogen atom or a cation of the same definition as above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having on average from 0.5 to 60 OE and / or OP units; ° the salts of C-8-C24, preferably C14-C20 saturated or unsaturated fatty acids, the sulfonated polycarboxylic acids described in GB-A-1 082 179; polyethoxycarboxylates, the cation being of the same definition as above, 0 alkylsulfosuccinates, monoesters or diesters of sulfosuccinates, such as sodium di-e
  • nonionic surfactants the following may be mentioned as examples: 0 the polyoxyalkylene derivatives of aliphatic or arylaliphatic alcohols in C8-C22 containing from 1 to 25 oxyalkylene units (oxyethylene, oxypropylene), polyoxyalkylene (polyethoxyethylenated, polyoxypropylene) alkylphenols whose alkyl substituent is C ⁇ -C-12 and containing from 5 to 25 oxyalkylene units, ° the alkylpolysaccharides having a hydrophobic group at C6-C3 0 , preferably at C- ⁇ o-C-16 and a polysaccharide group, for example polyglycoside, as hydrophilic group as well as from 1 to 3 sugar units, ° the alkylated derivatives of aminosugars, such as alkylglucamides produced by the amidation reaction of a fatty acid on N-methylglucamine, amine oxides such as alkyl oxides Cin-
  • amphoteric and zwitterionic surfactants the following are suitable: ° alkyldimethylbetaines, alkylamidopropyldimethylbetaines, alkyltrimethylsulfobetaines,
  • composition according to the invention can optionally comprise at least one filler.
  • fillers which can be used in the composition according to the invention, mention may be made, for example, of diatomaceous earth, clays such as bentonite, kaolin,
  • the amount of filler is preferably such that the composition remains substantially or completely water-soluble.
  • the amount of filler in the composition represents 0 to 50% by weight relative to the weight of the composition.
  • the amount of filler represents 0 to 30% by weight, and preferably 0 to 10% by weight relative to the same reference.
  • a more preferred embodiment of the invention consists in not using a filler.
  • the process for preparing the composition according to the invention consists in partially or totally eliminating, at least the water of crystallization, present in a mixture comprising at least one aforementioned mineral salt, at least a binder, optionally at least one surfactant, optionally at least one filler, and water which is at least in the form of water of crystallization.
  • This drying step during which the water, which is at least in the form of water of crystallization, is eliminated, makes it possible to adjust the absorption capacity of the granule, depending on whether one eliminates more or less the water of crystallization of the mineral salt.
  • drying operation also makes it possible to eliminate all or part, and preferably all, of the water capable of being supplied when the mixture to be dried is obtained, in addition to the water of crystallization.
  • the drying operation will be described below. This drying operation can advantageously be carried out in an oven, and preferably in a fluidized bed.
  • the drying advantageously, takes place in air, at atmospheric pressure or under reduced pressure.
  • the drying temperature depends on the nature of the compounds constituting the composition according to the invention. It must, moreover, be high enough to allow a departure of the water of crystallization of the mineral salt.
  • the temperature range can be between 60 and 150 ° C., preferably between 70 and 120 ° C.
  • the drying operation takes place on a mixture which can be obtained according to several advantageous variants.
  • a first variant consists in carrying out said drying on a mixture obtained in the following manner:
  • At least one mineral salt is mixed in anhydrous or partially hydrated form, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, with the quantity of water necessary and sufficient to hydrate totally said mineral salt,
  • granulation is carried out, more particularly using an aqueous solution, of the resulting mixture.
  • aqueous solution By partially hydrated is meant a mineral salt whose hydration rate is less than 80%.
  • the mixture passes intermediarily through a pasty state.
  • this operation there is a step of dissolving the salt (pasty medium) then hydration of the salt (reappearance of the powder).
  • This intermediate phase can advantageously contribute to improving the homogenization of the mixture.
  • the operation of adding water, in an amount necessary and sufficient to completely hydrate the mineral salt preferably takes place in a shearing mixer, such as in particular the turbospheres, Henry crusher, Stephan mixer, Lodige mixer.
  • a shearing mixer such as in particular the turbospheres, Henry crusher, Stephan mixer, Lodige mixer.
  • the addition of water may or may not be gradual.
  • the granulation step is carried out in a conventional manner (pan-granulation, extrusion).
  • the mixture in the form of particles is brought into contact with granulation water.
  • the granulation step is preferably carried out in the presence of an amount of water which makes it possible to obtain a mixture having a viscosity suitable for shaping.
  • This water content obviously depends on the nature of the mineral salt (s) chosen and on the nature of the material used. It can be determined without difficulty by those skilled in the art. However, by way of example, the amount of granulation water varies between 10 and 20% by weight relative to the weight of the composition for granulation by agglomeration. Granulation takes place in any suitable type of apparatus.
  • a second variant of preparation of the mixture intended to be dried consists in granulating at least one mineral salt in substantially hydrated form, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, and granulation water.
  • Substantially hydrated means that the degree of hydration of the mineral salt is greater than or equal to 80%.
  • Granulation takes place in a conventional manner (pan-granulation, extrusion).
  • the content of granulation water used is preferably such that a mixture is obtained having a viscosity suitable for shaping.
  • This water content obviously depends on the nature of the mineral salt (s) chosen, the material used and can be easily determined by those skilled in the art.
  • the amount of granulation water (or water of crystallization) varies between 10 and 20% by weight relative to the weight of the composition for granulation by agglomeration.
  • the third variant of preparation of the mixture intended to be dried consists in carrying out the following steps:. at least one mineral salt is mixed, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, with the quantity of water necessary to obtain a solution and / or a dispersion, • the solution and / or the dispersion are dried,. granulation of the resulting dried mixture is carried out.
  • the salt used can be in anhydrous or hydrated form, partially or completely.
  • composition according to the invention being substantially water-soluble, a solution is therefore obtained substantially, within the meaning of the present invention.
  • This drying step can take place using known techniques.
  • the drying is carried out by means of atomizers in which a spraying of the mixture is carried out in a hot atmosphere (spray-drying).
  • the atomization can be carried out by means of any sprayer known per se, for example by a spray nozzle of the sprinkler apple type or the like.
  • We can also use so-called turbine atomizers.
  • spraying techniques likely to be used in the present process, reference may be made in particular to the basic work by MASTERS entitled "SPRAY-DRYING" (second edition, 1976, Editions George Godwin - London).
  • the extremely short residence time (generally less than about 1/10 of a second) of the particles in the reactor has the advantage, inter alia, of limiting possible risks of overheating as a result of too long contact with the hot gases.
  • FIG. 1 of French patent application 2,431,321. The temperature of this drying is such that it does not degrade the constituent elements of the composition.
  • All the active ingredients are suitable insofar as they are in anhydrous form or include an amount of water insufficient to dissolve the composition according to the invention.
  • the formulation can comprise at least one active material which can be used in the food sector.
  • suitable active ingredients there may be mentioned flavorings, essential oils, vitamins (such as vitamins A or E), colorants, compounds preventing the formation of foams, such as polyethoxylated oils derived from palm, soybean oil, castor oil, rapeseed oil, corn oil, sunflower oil.
  • sucroglycerides mention may in particular be made of palm oil, lard, coconut oil, tallow, rapeseed oil or castor oil.
  • a procedure for the preparation of sucroglycerides is described in French patent application FR 2 463 512.
  • Polyglyceride esters of edible fatty acids esters of polypropylene glycol and edible fatty acids (monoesters or in mixture with diesters); polyethylene glycol ricinoleate; esters of polyethylene glycol and fatty acids derived from oils, such as soybean oil; glycerol and polyethylene glycol esters of fatty acids, such as tallow fatty acids; ethers of polyglycerol and alcohols obtained by reduction of oleic and palmitic acids; polycondensed partial castor fatty acid polyglycerol esters. Polysorbates can be advantageously used.
  • the formulation can comprise at least one active material usable in the pharmaceutical field, viruses, enzymes.
  • the formulation comprising the active material can be obtained by spraying or impregnating said active material, optionally in the presence of a dispersant / solvent, on the composition according to the invention. It should be noted, and this represents an additional advantage of the composition according to the invention, that this absorption step can be carried out directly after the preparation of the composition, or after storage of the composition.
  • the absorption is therefore carried out, in a conventional manner, by spraying, spraying or impregnating the active material on the composition according to the invention.
  • the active ingredient is in the form of a liquid, in dissolved form, in molten form.
  • a formulation according to the invention that is to say comprising the composition and at least one active material, as an additive (adjuvant ) to a more complex formulation.
  • the formulation according to the invention comprising the composition and at least one active ingredient
  • the other constituent elements of the more complex formulation it suffices to mix, during the very preparation of the complex formulation, using conventional means, the formulation according to the invention (comprising the composition and at least one active ingredient) with the other constituent elements of the more complex formulation.
  • the mixture is ground for the time necessary to obtain a powder.
  • Granulation of the powder is then carried out by adding 200 g of water.
  • a dry powder is obtained, indicating good impregnation of the granules.
  • the active material content is 40% relative to the total weight of the granules.

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Abstract

The invention relates to a substantially or partially hydrosoluble composition in the form of solid particles exhibiting an absorption capacity of up to 50 % and which can be obtained from at least one crystallizing mineral salt with at least one molecule and at least one organic polymer binder whereby the content thereof is less than 30 % of the weight of the composition, and drying is carried out whereby at least part of the water of crystallization is eliminated. The invention also relates to a method for the production of said composition, consisting of the following: as a result of a drying step, it is possible to fully or partially eliminate at least the water of crystallization present in the mixture comprising the above-mentioned mineral salt, the binder and the water which also exists partially in the form of the water of crystallization. The invention further relates to a formulation comprising an active substance that is absorbed on the above-mentioned composition and a method for producing said formulation by atomization or impregnation of the active substance.

Description

COMPOSITION A BASE D'UN SEL MINERAL SUBSTANTIELLEMENT OU TOTALEMENT HYDROSOLUBLE, FORMULATION LA COMPRENANT, ET COMPOSITION BASED ON SUBSTANTIALLY OR TOTALLY WATER-SOLUBLE MINERAL SALT, FORMULATION COMPRISING SAME, AND
LEURS PREPARATIONSTHEIR PREPARATIONS
La présente invention a pour objet une composition sous forme de particules solides, substantiellement ou totalement hydrosoluble, comprenant un sel minéral cristallisant avec au moins une molécule d'eau, un liant. La composition est susceptible d'être obtenue par une opération de séchage éliminant au moins en partie l'eau de cristallisation dudit sel.The subject of the present invention is a composition in the form of solid particles, substantially or completely water-soluble, comprising a mineral salt crystallizing with at least one molecule of water, a binder. The composition can be obtained by a drying operation at least partially eliminating the water of crystallization of said salt.
Elle a de même pour objet une formulation comprenant au moins une matière active absorbée sur la composition précitée, et le procédé de préparation de ladite formulation.It also relates to a formulation comprising at least one active material absorbed on the aforementioned composition, and the process for the preparation of said formulation.
Dans de nombreux domaines techniques, on a cherché à préparer des poudres coulables à base de matières actives liquides ou solubilisées. Parmi les possibilités figurent celle consistant à former un grain dans lequel la matière active est absorbée.In many technical fields, attempts have been made to prepare flowable powders based on liquid or solubilized active materials. Among the possibilities is that of forming a grain in which the active material is absorbed.
L'un des problèmes à résoudre a trait à la capacité d'absorption du grain. En effet, cette dernière doit être la plus élevée possible de manière à obtenir, après absorption, une concentration la plus élevée possible en matière active. Une autre difficulté, qui se trouve être la conséquence d'une capacité d'absorption élevée, est la résistance à l'attrition du grain. En effet, plus la capacité d'absorption est grande, plus la porosité est élevée, moins la résistance à l'attrition est importante, ce qui laisse présager des difficultés au stockage par exemple, du grain seul, mais éventuellement aussi, de la formulation complète. Dans le domaine de la détergence, on connaît des procédé de préparation comprenant deux étapes, la première consistant à préparer le grain seul, et la seconde à pulvériser sur ce dernier, la matière active, qui se trouve être bien souvent, un tensioactif non ionique.One of the problems to be resolved relates to the absorption capacity of the grain. Indeed, the latter must be as high as possible so as to obtain, after absorption, the highest possible concentration of active material. Another difficulty, which happens to be the consequence of a high absorption capacity, is the resistance to grain attrition. In fact, the greater the absorption capacity, the higher the porosity, the lower the attrition resistance, which suggests difficulties in storing, for example, the grain alone, but possibly also the formulation complete. In the detergency field, there are known preparation processes comprising two stages, the first consisting in preparing the grain alone, and the second in spraying on the latter, the active material, which very often happens to be a nonionic surfactant. .
Le grain est obtenu par atomisation d'un mélange comprenant notamment un sel du type silicate, phosphate, et comprenant le cas échéant, d'autres additifs comme des agents anti-redéposition. La matière active, éventuellement elle aussi additivée, est ensuite pulvérisée sur les grains obtenus.The grain is obtained by atomization of a mixture comprising in particular a salt of the silicate, phosphate type, and comprising, where appropriate, other additives such as anti-redeposition agents. The active ingredient, optionally also additive, is then sprayed onto the grains obtained.
Si des avantages existent avec un tel procédé, il n'en reste pas moins que la capacité d'absorption du granulé reste un peu faible. Certes il existe, dans l'art antérieur, des procédés de- préparation de composés très absorbants, comme par exemple le carbonate de sodium. Les procédés consistent, à partir de carbonate de sodium décahydrate, à mettre en œuvre un traitement thermique très contrôlé, dont le but est d'éliminer les 10 moles d'eau présentes, créant de ce fait une porosité importante dans les particules. Cependant, ces dernières ont une taille qui ne dépasse pas 10 μm en moyenne. Par conséquent, si leur capacité d'absorption est très importante, de telles particules ne sont pas toujours souhaitées, car elle nécessitent des précautions d'utilisation du fait de leur caractère pulvérulent. La présente invention a donc pour objet de proposer une composition, qui puisse servir de matrice à une matière active destinée y être absorbée, composition qui soit totalement ou substantiellement hydrosoluble, très absorbante et non pulvérulente.If advantages exist with such a process, the fact remains that the absorption capacity of the granule remains somewhat low. Certainly there exist, in the prior art, processes for the preparation of highly absorbent compounds, such as for example sodium carbonate. The processes consist, starting from sodium carbonate decahydrate, in implementing a very controlled heat treatment, the aim of which is to eliminate the 10 moles of water present, creating therefore a large porosity in the particles. However, the latter have a size which does not exceed 10 μm on average. Consequently, if their absorption capacity is very high, such particles are not always desired, because they require precautions for use due to their pulverulent nature. The object of the present invention is therefore to provide a composition which can serve as a matrix for an active material intended to be absorbed therein, a composition which is totally or substantially water-soluble, very absorbent and not pulverulent.
Il est à noter que par substantiellement, on entend au sens de la présente invention, que plus de 50 % de ladite composition soit solubilisée dans l'eau, plus particulièrement, au moins 80 %, de préférence au moins 90 %.It should be noted that by substantially, within the meaning of the present invention, it is meant that more than 50% of said composition is dissolved in water, more particularly, at least 80%, preferably at least 90%.
Ainsi, un premier objet de l'invention est constitué par une composition, sous forme de particules solides, substantiellement ou totalement hydrosoluble, dont la capacité d'absorption d'au moins une matière active peut atteindre 50 % en poids, correspondant au rapport en poids de la matière active à la somme de la composition et de la matière active ; ladite composition étant susceptible d'être obtenue à partir d'au moins un sel minéral cristallisant avec au moins une molécule d'eau, d'au moins un liant organique polymérique dont la teneur est inférieure à 30 % en poids de la composition, éventuellement d'au moins un tensioactif, éventuellement d'au moins une charge, ladite composition étant susceptible d'être obtenue par séchage éliminant au moins une partie de l'eau de cristallisation.Thus, a first object of the invention consists of a composition, in the form of solid particles, substantially or completely water-soluble, the absorption capacity of at least one active material of which can reach 50% by weight, corresponding to the ratio of weight of the active ingredient at the sum of the composition and the active ingredient; said composition being capable of being obtained from at least one mineral salt crystallizing with at least one molecule of water, from at least one organic polymeric binder whose content is less than 30% by weight of the composition, optionally at least one surfactant, optionally at least one filler, said composition being capable of being obtained by drying eliminating at least part of the water of crystallization.
Un second objet de l'invention est relatif à un procédé de préparation de ladite composition dans lequel on élimine partiellement ou totalement, au moins l'eau de cristallisation, présente dans un mélange comprenant au moins un sel minéral précité, au moins un liant organique polymérique, éventuellement au moins un tensioactif, éventuellement au moins une charge, et de l'eau qui se trouve au moins sous la forme d'eau de cristallisation.A second subject of the invention relates to a process for the preparation of said composition in which at least partially or completely, at least the water of crystallization is removed, present in a mixture comprising at least one aforementioned mineral salt, at least one organic binder polymer, optionally at least one surfactant, optionally at least one filler, and water which is at least in the form of water of crystallization.
Un autre objet de l'invention est relatif à une formulation comprenant au moins une matière active absorbée sur la composition selon l'invention.Another subject of the invention relates to a formulation comprising at least one active material absorbed on the composition according to the invention.
Enfin, un dernier objet de l'invention concerne la préparation de ladite formulation ; procédé dans lequel on effectue une pulvérisation ou une imprégnation de la matière active, sous la forme d'un liquide, sur la composition selon l'invention.Finally, a final object of the invention relates to the preparation of said formulation; process in which a spraying or impregnation of the active material is carried out, in the form of a liquid, on the composition according to the invention.
Ainsi que cela a été mentionné auparavant, la composition selon l'invention présente l'avantage d'avoir une capacité à l'absorption très élevée. En effet, il est possible d'absorber sur la composition une quantité de matière active qui représente le poids de la composition. En termes différents, la composition selon l'invention présente une absorption qui peut être aussi élevée que 50 % (rapport en poids de la matière active à la somme de la composition et de la matière active). La capacité d'absorption est mesurée par rapport au Rhodasurf ID 79, qui est un tensioactif non ionique (alcool isodécylique comprenant 7 motifs oxyde d'éthylène - commercialisé par Rhodia Chimie). Le test consiste à mettre la composition en contact avec le tensioactif, à température ambiante, progressivement et sous agitation, jusqu'à ce que le mélange prenne un aspect collant (le mélange solide ne s'écoule plus de manière fluide - non free-flowing). On évalue alors la quantité de tensioactif ajouté.As mentioned previously, the composition according to the invention has the advantage of having a very high absorption capacity. Indeed, it is possible to absorb on the composition an amount of active material which represents the weight of the composition. In different terms, the composition according to the invention has an absorption which can be as high as 50% (ratio by weight of the active material to the sum of the composition and the active material). The absorption capacity is measured relative to Rhodasurf ID 79, which is a nonionic surfactant (isodecyl alcohol comprising 7 ethylene oxide units - sold by Rhodia Chimie). The test consists in bringing the composition into contact with the surfactant, at room temperature, gradually and with stirring, until the mixture takes on a tacky appearance (the solid mixture no longer flows fluidly - not free-flowing ). The amount of surfactant added is then evaluated.
Du fait de son pH, la composition selon l'invention présente l'avantage d'être compatible avec de nombreux domaines d'utilisation aussi variés que la détergence, le domaine alimentaire, l'industrie pharmaceutique, l'industrie agrochimique. Par ailleurs, la composition selon l'invention est constituée de particules poreuses non pulvérulentes, dont la taille est suffisante pour ne pas poser de problèmes de manipulation.Because of its pH, the composition according to the invention has the advantage of being compatible with many fields of use as varied as detergency, the food sector, the pharmaceutical industry, the agrochemical industry. Furthermore, the composition according to the invention consists of non-pulverulent porous particles, the size of which is sufficient so as not to pose handling problems.
De plus, la résistance à l'attrition des particules de la composition est améliorée, ce qui présente des avantages évidents pour le stockage et la manipulation de la composition.In addition, the attrition resistance of the particles of the composition is improved, which has obvious advantages for the storage and handling of the composition.
La composition selon l'invention peut être employée pour obtenir des formulations solides alors que la matière active est liquide, fondue ou solubilisée.The composition according to the invention can be used to obtain solid formulations while the active material is liquid, molten or dissolved.
La composition selon l'invention présente l'avantage de pouvoir mélanger dans un même conditionnement des substances qui auraient été incompatibles en mélange liquide (si les substances sont chimiquement réactives entre elles, par exemple).The composition according to the invention has the advantage of being able to mix, in the same packaging, substances which would have been incompatible in a liquid mixture (if the substances are chemically reactive with one another, for example).
En outre, la composition selon l'invention peut être adaptée en fonction des matières actives pour lesquelles elle servira de support. Ainsi, la composition selon l'invention peut être avantageusement employée pour des matières actives sensibles au pH. Notons comme caractéristique avantageuse supplémentaire de la composition selon l'invention, qu'elle contribue à faciliter l'emploi de la formulation ultérieure qui la contient. En effet, la composition selon l'invention confère à ladite formulation, des propriétés de dissolution plus ou moins rapide et surtout, ajustable.In addition, the composition according to the invention can be adapted according to the active materials for which it will serve as a support. Thus, the composition according to the invention can be advantageously used for active materials sensitive to pH. It should be noted as an additional advantageous characteristic of the composition according to the invention that it contributes to facilitating the use of the subsequent formulation which contains it. In fact, the composition according to the invention gives said formulation, more or less rapid and above all, adjustable dissolution properties.
La dureté du granulé (résistance à l'attrition), sa capacité d'absorption, son pH, peuvent aussi, et cela représente des caractéristiques intéressantes de la composition de l'invention, être ajustés en fonction des utilisations ultérieures des formulations qui la comprennent.The hardness of the granule (resistance to attrition), its absorption capacity, its pH, can also, and this represents advantageous characteristics of the composition of the invention, be adjusted according to the subsequent uses of the formulations which comprise it. .
Enfin, le procédé de préparation de la composition selon l'invention est simple et permet d'obtenir des formes diverses de particules. Mais d'autres caractéristiques et avantages de la présente invention apparaîtront plus clairement à la lecture de la description et des exemples qui vont suivre.Finally, the process for preparing the composition according to the invention is simple and makes it possible to obtain various forms of particles. However, other characteristics and advantages of the present invention will appear more clearly on reading the description and the examples which follow.
Ainsi que cela a été indiqué précédemment, la composition selon l'invention comprend un sel minéral cristallisant avec au moins une molécule d'eau. Plus particulièrement le sel minéral est choisi parmi les phosphates de métal alcalin, le carbonate de métal alcalin, le sulfate de métal alcalin ou d'aluminium, le borate de métal alcalin, les sels d'aluminium, le chlorure de magnésium, ou leurs mélanges. En ce qui concerne tout particulièrement les phosphates de métal alcalin, conviennent à la mise en œuvre de l'invention les pyrophosphate, tripolyphosphate, phosphate mono-, di- ou tri-sodique, hexamétaphosphate, ou leurs mélanges.As indicated above, the composition according to the invention comprises an inorganic salt crystallizing with at least one molecule of water. More particularly the mineral salt is chosen from alkali metal phosphates, alkali metal carbonate, alkali metal or aluminum sulfate, alkali metal borate, aluminum salts, magnesium chloride, or mixtures thereof . As regards very particularly the alkali metal phosphates, the pyrophosphate, tripolyphosphate, mono-, di- or tri-sodium phosphate, hexametaphosphate, or mixtures thereof, are suitable for implementing the invention.
De préférence, la composition selon l'invention comprend à titre de sel minéral au moins un sel choisi parmi les phosphates, et notamment ceux mentionnés, ainsi que les carbonates de métal alcalin, et plus particulièrement de sodium.Preferably, the composition according to the invention comprises as mineral salt at least one salt chosen from phosphates, and in particular those mentioned, as well as the alkali metal carbonates, and more particularly sodium.
De préférence, les sels minéraux mis en œuvre pour la préparation de la composition selon l'invention ne comprennent pas de tripolyphosphate seul. Selon un mode avantageux, les sels mis en œuvre ne comprennent de tripolyphosphate ni seul ni combiné à un ou plusieurs autres sels. La quantité en sel minéral représente 50 à moins de 100 % en poids de la composition. Selon un mode de réalisation particulier de l'invention, la quantité en sel minéral est comprise entre 70 et moins de 100 % en poids par rapport à la même référence. De préférence, la quantité en sel minéral est comprise entre 85 et moins de 100 % en poids par rapport à la même référence. La composition selon l'invention comprend en outre, au moins un liant organique polymérique.Preferably, the mineral salts used for the preparation of the composition according to the invention do not comprise tripolyphosphate alone. According to an advantageous mode, the salts used do not comprise tripolyphosphate either alone or combined with one or more other salts. The amount of mineral salt represents 50 to less than 100% by weight of the composition. According to a particular embodiment of the invention, the amount of mineral salt is between 70 and less than 100% by weight relative to the same reference. Preferably, the amount of mineral salt is between 85 and less than 100% by weight relative to the same reference. The composition according to the invention also comprises at least one organic polymeric binder.
Parmi les composés susceptibles d'être utilisés, seuls ou en combinaison, en tant que liant, on peut citer les monosaccharides, les oligosaccharides, les polymères naturels du type des polysaccharides d'origine animale, végétale, bactérienne, les polymères synthétiques du type des polyalkyleneglycols, de l'alcool polyvinylique, des polymères d'acide (méth)acrylique ou copolymère d'acide (méth)acrylique et d'isobutylene ou de diisobutylène, des acides polyacryliques et leurs sels, des copolymères d'anhydride (ou acide) maleique et d'isobutylene ou de diisobutylène, et leurs sels, ainsi que leurs mélanges. Le lactose, le saccharose, seuls ou en mélange, représentent des exemples possibles de liants choisis parmi les monosaccharides et oligosaccharides.Among the compounds capable of being used, alone or in combination, as a binder, mention may be made of monosaccharides, oligosaccharides, natural polymers of the type of polysaccharides of animal, plant, bacterial origin, synthetic polymers of the type of polyalkyleneglycols, polyvinyl alcohol, polymers of (meth) acrylic acid or copolymer of (meth) acrylic acid and isobutylene or diisobutylene, polyacrylic acids and their salts, anhydride (or acid) copolymers maleique and isobutylene or diisobutylene, and their salts, and mixtures thereof. Lactose and sucrose, alone or as a mixture, represent possible examples of binders chosen from monosaccharides and oligosaccharides.
En ce qui concerne les polymères naturels du type des polysaccharides d'origine animale, végétale, bactérienne, on peut citer à titre d'exemple non limitatif, la gomme xanthane, le guar et dérivés (tels que l'hydroxypropyl guar par exemple), les polydextroses, ou leurs combinaisons.With regard to natural polymers of the type of polysaccharides of animal, vegetable or bacterial origin, non-limiting examples that may be mentioned are xanthan gum, guar and derivatives (such as hydroxypropyl guar for example), polydextroses, or combinations thereof.
Parmi les polymères synthétiques, conviennent notamment, seuls ou en mélange, les polyéthylèneglycols, polypropylèneglycols, polybutylèneglycols, les copolymères de polyéthylène- et polypropylène- glycols, l'alcool polyvinylique, les polymères d'acide (méth)acrylique ou copolymères d'acide (méth)acrylique et d'isobutylene ou de diisobutylène, ainsi que leurs sels.Among the synthetic polymers, polyethylene glycols, polypropylene glycols, polybutylene glycols, polyethylene- and polypropylene glycol copolymers, polyvinyl alcohol, acid polymers are especially suitable, alone or as a mixture. (meth) acrylic or copolymers of (meth) acrylic acid and isobutylene or diisobutylene, as well as their salts.
Conviennent aussi particulièrement, et cela représente un mode de réalisation préféré de l'invention, les polymères d'acide acrylique tels que le Geropon® HB, ainsi que les copolymères d'anhydride (ou d'acide) maleique et de diisobutylène.Also particularly suitable, and this represents a preferred embodiment of the invention, acrylic acid polymers such as Geropon® HB, as well as copolymers of maleic anhydride (or acid) and diisobutylene.
Ces copolymères peuvent se trouver sous la forme acide ou bien sous une forme de sel de métal alcalin ou d'ammonium de type N(R)4 +, avec R, identiques ou différents, représentant des atomes d'hydrogène, ou des radicaux hydrocarbonés en C1-C4. De préférence, le copolymère se trouve sous forme de sel de sodium. Ces copolymères sont des composés bien connus et sont notamment commercialisés sous la dénomination GEROPON® T 36(Rhodia).These copolymers can be in the acid form or in the form of an alkali metal or ammonium salt of type N (R) 4 + , with R, identical or different, representing hydrogen atoms, or hydrocarbon radicals in C1-C4. Preferably, the copolymer is in the form of the sodium salt. These copolymers are well known compounds and are in particular marketed under the name GEROPON® T 36 (Rhodia).
La quantité d'agent liant est plus particulièrement comprise entre 0 exclu et 30 % en poids de la composition selon l'invention. Selon un mode de réalisation particulier de l'invention, la quantité en liant est comprise entre 0 exclu et 15 % en poids par rapport à la même référence. Cependant, selon une variante très préférentielle de l'invention, la teneur en liant est comprise entre 0,5 et 15 % en poids par rapport à la composition.The amount of binding agent is more particularly between 0 excluded and 30% by weight of the composition according to the invention. According to a particular embodiment of the invention, the amount of binder is between 0 excluded and 15% by weight relative to the same reference. However, according to a very preferred variant of the invention, the content of binder is between 0.5 and 15% by weight relative to the composition.
Il est à noter que si la composition selon l'invention ne comprend que le sel minéral et le liant polymérique, les teneurs respectives en ces composés sont telles que l'ensemble représente 100% en poids. Selon un mode de réalisation de l'invention, le rapport pondéral entre le sel minéral et le liant est compris entre 99,5/0,5 et 60/40. Plus particulièrement ledit rapport pondéral est compris entre 99,5/05 et 70/30, de préférence entre 99,5/0,5 et 85/15.It should be noted that if the composition according to the invention only comprises the mineral salt and the polymeric binder, the respective contents of these compounds are such that the whole represents 100% by weight. According to one embodiment of the invention, the weight ratio between the mineral salt and the binder is between 99.5 / 0.5 and 60/40. More particularly, said weight ratio is between 99.5 / 05 and 70/30, preferably between 99.5 / 0.5 and 85/15.
La composition selon l'invention peut de même comprendre, le cas échéant, au moins un tensioactif. Sans vouloir être limité par une quelconque théorie, le tensioactif, lorsqu'il est présent, a deux rôles, celui d'optimiser le mouillage du sel minéral et du liant, et celui d'optimiser la dispersion de la matière active lors de son utilisation.The composition according to the invention can likewise comprise, if necessary, at least one surfactant. Without wishing to be limited by any theory, the surfactant, when it is present, has two roles, that of optimizing the wetting of the mineral salt and of the binder, and that of optimizing the dispersion of the active material during its use .
Tous les tensioactifs peuvent convenir à l'invention, dans la mesure où ils sont compatibles avec la matière active Ainsi, on peut mettre en oeuvre des tensioactifs anioniques, non ioniques, cationiques, zwittérioniques ou amphotères. Parmi les tensioactifs anioniques, on peut citer à titre d'exemple : ° Les polymères dérivés de la lignine comme les lignosulfonates de sodium ou de calcium ; ° les alkylesters sulfonates de formule R-CH(Sθ3M)-COOR', où R représente un radical alkyle en C-8-C20, de préférence en C10-C-16, R" un radical alkyle en Ci-Cβ, de préférence en C1-C3 et M un cation alcalin (sodium, potassium, lithium), ammonium substitué ou non substitué (méthyl-, diméthyl-, triméthyl-, tetraméthylammonium, diméthylpiperidinium ...) ou dérivé d'une alcanolamine (monoéthanolamine, diéthanolamine, triéthanolamine ...). On peut citer tout particulièrement les méthyl ester sulfonates dont le radical R est en C14-C16 ; les alkylsulfonates primaires ou secondaires en C8-C20 ; les alkylarylsulfonates comme l'isopropylnaphtalène sulfonate de sodium, commercialisé sous le nom Supragil WP® ; les alkylbenzènesulfonates en C9-C20 ; les méthylnaphtalène sulfonate de sodium condensés comme le Supragil MNS90®, les sulfonates de paraffine. les alkylsulfates de formule ROSO3M, où R représente un radical alkyle ou hydroxyalkyle en C-10-C24, de préférence en C12-C20 et tout particulièrement en C12-C18, M représentant un atome d'hydrogène ou un cation de même définition que ci-dessus, ainsi que leurs dérivés éthoxylénés (OE) et/ou propoxylénés (OP), présentant en moyenne de 0,5 à 6 motifs, de préférence de 0,5 à 3 motifs OE et/ouAll the surfactants can be suitable for the invention, insofar as they are compatible with the active material. Thus, anionic, nonionic, cationic, zwitterionic or amphoteric surfactants can be used. Among the anionic surfactants that may be mentioned by way of example: ° Polymers derived from lignin, such as sodium or calcium lignosulfonates; ° the alkyl esters sulfonates of formula R-CH (Sθ3M) -COOR ', where R represents an alkyl radical in C-8-C20, preferably in C10-C-16, R "an alkyl radical in Ci-Cβ, preferably in C1-C3 and M an alkali cation (sodium, potassium, lithium), substituted or unsubstituted ammonium (methyl-, dimethyl-, trimethyl-, tetramethylammonium, dimethylpiperidinium ...) or derived from an alkanolamine (monoethanolamine, diethanolamine, triethanolamine ...). Mention may very particularly be made of methyl ester sulfonates, the radical R of which is C14-C16; primary or secondary C8-C20 alkylsulfonates; alkylaryl sulfonates such as sodium isopropyl naphthalene sulfonate, sold under the name ® Supragil WP; C9-C20 alkylbenzenesulfonates; condensed sodium methylnaphthalene sulfonate such as Supragil MNS90®, paraffin sulfonates. alkyl sulphates of formula ROSO3M, where R represents a C 10 -C 24, preferably C 12 -C 20 and especially C 12 -C 18 alkyl or hydroxyalkyl radical, M representing a hydrogen atom or a cation of the same definition as ci above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having on average from 0.5 to 6 units, preferably from 0.5 to 3 OE units and / or
OP ; les sulfates d'alkylglycosides ; les alkylalryl sulfates, comme les mono-, di- ou tri-tristyryl phénols polyoxyalkylènesOP; alkyl glycoside sulfates; alkylalryl sulfates, such as mono-, di- or tri-tristyryl polyoxyalkylene phenols
(OE et/ou OP); éventuellement neutralisés en totalité ou partiellement ; les alkylamides sulfates de formule RCONHROSO3M où R représente un radical alkyle en C-2-C22, de préférence en C6-C20, R' un radical alkyle en C2-C3, M représentant un atome d'hydrogène ou un cation de même définition que ci-dessus, ainsi que leurs dérivés éthoxylénés (OE) et/ou propoxylénés (OP), présentant en moyenne de 0,5 à 60 motifs OE et/ou OP ; ° les sels d'acides gras saturés ou insaturés en C-8-C24, de préférence en C14-C20, les acides polycarboxyliques sulfonés décrits dans GB-A-1 082 179 ; les polyéthoxycarboxylates, le cation étant de même définition que précédemment , 0 les alkylsulfosuccinates, les monoesters ou diesters de sulfosuccinates, comme le di-éthyl-2-hexyl sulfosuccinate de sodium, ° les N-acyl sarcosinates, les N-acyl N-alkyl taurates ; ° les alkyliséthionates ; a les alkylsuccinamates ; ° les alkylphosphates.(OE and / or OP); possibly neutralized in whole or in part; the alkylamides sulfates of formula RCONHROSO3M where R represents an alkyl radical in C-2-C22, preferably in C6-C20, R 'an alkyl radical in C2-C3, M representing a hydrogen atom or a cation of the same definition as above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having on average from 0.5 to 60 OE and / or OP units; ° the salts of C-8-C24, preferably C14-C20 saturated or unsaturated fatty acids, the sulfonated polycarboxylic acids described in GB-A-1 082 179; polyethoxycarboxylates, the cation being of the same definition as above, 0 alkylsulfosuccinates, monoesters or diesters of sulfosuccinates, such as sodium di-ethyl-2-hexyl sulfosuccinate, ° N-acyl sarcosinates, N-acyl N-alkyl taurates; ° alkylisethionates; a alkylsuccinamates; ° alkylphosphates.
Parmi les tensioactifs non-ioniques, on peut mentionner comme exemple : 0 les dérivés polyoxyalkylènes d'alcools aliphatiques ou arylaliphatiques en C8-C22 contenant de 1 à 25 motifs oxyalkylenes (oxyéthylène, oxypropyléné), les alkylphénols polyoxyalkylènes (polyéthoxyéthylénés, polyoxypropylénés, polyoxybutylénés) dont le substituant alkyle est en Cβ-C-12 et contenant de 5 à 25 motifs oxyalkylenes, ° les alkylpolysaccharides présentant un groupement hydrophobe en C6-C30, de préférence en C-ιo-C-16 et un groupement polysaccharide, par exemple polyglycoside, comme groupement hydrophile ainsi que de 1 à 3 unités sucre, ° les dérivés alkylés d'aminosucres, comme les alkylglucamides produits par la réaction d'amidification d'un acide gras sur la N-méthylglucamine, les oxydes d'aminés tels que les oxydes d'alkyl Cin-C-is diméthylamines, les oxydes d'alkoxy C8-C22 éthyl dihydroxy éthylamines, les alkylglucamides, les glycérolamides dérivés de N-alkylamines (US-A-5,223,179 et FR-A-1 ,585,966), ° les amides d'acides gras en C8-C20, les acides gras éthoxylés, les amides gras éthoxylés, les aminés éthoxylées.Among the nonionic surfactants, the following may be mentioned as examples: 0 the polyoxyalkylene derivatives of aliphatic or arylaliphatic alcohols in C8-C22 containing from 1 to 25 oxyalkylene units (oxyethylene, oxypropylene), polyoxyalkylene (polyethoxyethylenated, polyoxypropylene) alkylphenols whose alkyl substituent is Cβ-C-12 and containing from 5 to 25 oxyalkylene units, ° the alkylpolysaccharides having a hydrophobic group at C6-C3 0 , preferably at C-ιo-C-16 and a polysaccharide group, for example polyglycoside, as hydrophilic group as well as from 1 to 3 sugar units, ° the alkylated derivatives of aminosugars, such as alkylglucamides produced by the amidation reaction of a fatty acid on N-methylglucamine, amine oxides such as alkyl oxides Cin-C-is dimethylamines, alkoxy oxides C8-C22 ethyl dihydroxy ethylamines, alkylglucamides, glycerolamides derived from N-alkylamines (US-A-5,223,179 and FR-A-1, 585.966), ° C8-C20 fatty acid amides, ethoxylated fatty acids, fatty amides ethoxylated, ethoxylated amines.
Comme tensioactifs cationiques, on peut citer tout particulièrement les halogénures d'alkyldiméthylammonium.As cationic surfactants, mention may very particularly be made of alkyl dimethyl ammonium halides.
A titre de tensioactifs amphotères et zwitterioniques, conviennent : ° les alkyldiméthylbétaïnes, les alkylamidopropyldiméthylbétaïnes, les alkyltriméthyl- sulfobétaïnes,As amphoteric and zwitterionic surfactants, the following are suitable: ° alkyldimethylbetaines, alkylamidopropyldimethylbetaines, alkyltrimethylsulfobetaines,
° les alkylsultaïnes, les alkylamidopropylhydroxysultaïnes,° alkylsultaines, alkylamidopropylhydroxysultaines,
° les produits de condensation d'acides gras sur les protéines ou les hydrolysats de protéines, ° les dérivés amphotères des alkylpolyamines comme l'Amphionic XL® commercialisé par Rhodia, Ampholac 7T/X® et Ampholac 7C/X® commercialisés par Berol Nobel,° the condensation products of fatty acids on proteins or protein hydrolysates, ° amphoteric derivatives of alkylpolyamines such as Amphionic XL ® marketed by Rhodia, Ampholac 7T / X ® and Ampholac 7C / X ® marketed by Berol Nobel,
° les dérivés d'imidazoiine tels que les alkylamphoacétates, alkylamphodiacétates, alkylamphopropionates, alkylamphodipropionates. Les tensioactifs précités peuvent être utilisés seuls ou en mélange. La quantité de tensioactif est comprise plus particulièrement entre 0 et 15 % en poids par rapport au poids de la composition. Plus particulièrement, elle est comprise entre 0 et 5 % en poids par rapport à la même référence.° imidazole derivatives such as alkylamphoacetates, alkylamphodiacetates, alkylamphopropionates, alkylamphodipropionates. The above surfactants can be used alone or as a mixture. The amount of surfactant is more particularly between 0 and 15% by weight relative to the weight of the composition. More particularly, it is between 0 and 5% by weight relative to the same reference.
La composition selon l'invention peut éventuellement comprendre au moins une charge.The composition according to the invention can optionally comprise at least one filler.
Parmi les charges utilisables dans la composition selon invention, on peut citer par exemple les terres de diatomées, les argiles comme la bentonite, le kaolin,Among the fillers which can be used in the composition according to the invention, mention may be made, for example, of diatomaceous earth, clays such as bentonite, kaolin,
Pattapulgite, les zéolithes ; le carbonate de calcium, le talc, le mica, les silices précipitées, les silicates de métaux alcalins ou alcalino-terreux, la perlite, le charbon, la lignite. Ces composés peuvent être présents seuls ou en mélanges.Pattapulgite, zeolites; calcium carbonate, talc, mica, precipitated silicas, silicates of alkali or alkaline earth metals, perlite, coal, lignite. These compounds can be present alone or in mixtures.
La quantité de charge est de préférence telle que la composition reste substantiellement ou totalement hydrosoluble.The amount of filler is preferably such that the composition remains substantially or completely water-soluble.
Plus particulièrement, la quantité de charge dans la composition représente 0 à 50 % en poids par rapport au poids de la composition. Selon un mode de réalisation particulier de l'invention, la quantité de charge représente 0 à 30 % en poids, et de préférence, 0 à 10 % en poids par rapport à la même référence. Un mode de réalisation plus préféré de l'invention consiste à ne pas utiliser de charge.More particularly, the amount of filler in the composition represents 0 to 50% by weight relative to the weight of the composition. According to a particular embodiment of the invention, the amount of filler represents 0 to 30% by weight, and preferably 0 to 10% by weight relative to the same reference. A more preferred embodiment of the invention consists in not using a filler.
La somme de tous les composés précités (sel minéral, liant, tensioactif, charge), représente 100 % en poids de la composition. Le procédé de préparation de la composition selon l'invention va maintenant être décrit plus en détails.The sum of all the above-mentioned compounds (mineral salt, binder, surfactant, filler) represents 100% by weight of the composition. The process for preparing the composition according to the invention will now be described in more detail.
Ainsi que cela a été mentionné plus haut, le procédé de préparation de la composition selon l'invention, consiste à éliminer partiellement ou totalement, au moins l'eau de cristallisation, présente dans un mélange comprenant au moins un sel minéral précité, au moins un liant, éventuellement au moins un tensioactif, éventuellement au moins une charge, et de l'eau qui se trouve au moins sous la forme d'eau de cristallisation.As mentioned above, the process for preparing the composition according to the invention consists in partially or totally eliminating, at least the water of crystallization, present in a mixture comprising at least one aforementioned mineral salt, at least a binder, optionally at least one surfactant, optionally at least one filler, and water which is at least in the form of water of crystallization.
Cette étape de séchage, durant laquelle l'eau, qui se présente au moins sous la forme d'eau de cristallisation, est éliminée, permet d'ajuster la capacité d'absorption du granulé, selon que l'on élimine plus ou moins l'eau de cristallisation du sel minéral.This drying step, during which the water, which is at least in the form of water of crystallization, is eliminated, makes it possible to adjust the absorption capacity of the granule, depending on whether one eliminates more or less the water of crystallization of the mineral salt.
Il est à noter que l'opération de séchage permet aussi d'éliminer en tout ou en partie, et de préférence en totalité, l'eau susceptible d'être apportée lors de l'obtention du mélange à sécher, en plus de l'eau de cristallisation. L'opération de séchage sera décrite dans la suite. Cette opération de séchage peut être avantageusement mise en œuvre dans une étuve, et de préférence en lit fluidisé.It should be noted that the drying operation also makes it possible to eliminate all or part, and preferably all, of the water capable of being supplied when the mixture to be dried is obtained, in addition to the water of crystallization. The drying operation will be described below. This drying operation can advantageously be carried out in an oven, and preferably in a fluidized bed.
Le séchage, avantageusement, a lieu sous air, à pression atmosphérique ou sous pression réduite.The drying, advantageously, takes place in air, at atmospheric pressure or under reduced pressure.
La température de séchage dépend de la nature des composés constituants la composition selon l'invention. Elle doit, de plus, être suffisamment élevée pour permettre un départ de l'eau de cristallisation du sel minéral.The drying temperature depends on the nature of the compounds constituting the composition according to the invention. It must, moreover, be high enough to allow a departure of the water of crystallization of the mineral salt.
Sans intention de s'y limiter, la gamme de température peut, être comprise entre 60 et 150°C, de préférence entre 70 et 120°C.Without intending to be limited thereto, the temperature range can be between 60 and 150 ° C., preferably between 70 and 120 ° C.
L'opération de séchage a lieu sur un mélange qui peut être obtenu selon plusieurs variantes avantageuses.The drying operation takes place on a mixture which can be obtained according to several advantageous variants.
Une première variante consiste à effectuer ledit séchage sur un mélange obtenu de la manière suivante :A first variant consists in carrying out said drying on a mixture obtained in the following manner:
. on mélange au moins un sel minéral sous forme anhydre ou partiellement hydratée, en présence d'au moins un liant, éventuellement d'au moins un tensioactif, éventuellement d'au moins une charge, avec la quantité d'eau nécessaire et suffisante pour hydrater totalement ledit sel minéral,. at least one mineral salt is mixed in anhydrous or partially hydrated form, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, with the quantity of water necessary and sufficient to hydrate totally said mineral salt,
. on effectue une granulation, plus particulièrement à l'aide d'une solution aqueuse, du mélange résultant. Par partiellement hydraté, on entend désigner un sel minéral dont le taux d'hydratation est inférieur à 80 %.. granulation is carried out, more particularly using an aqueous solution, of the resulting mixture. By partially hydrated is meant a mineral salt whose hydration rate is less than 80%.
Selon cette première variante, le mélange passe intermédiairement par un état pâteux. En effet, pendant cette opération, on passe par une étape de dissolution du sel (milieu pâteux) puis par une hydratation du sel (réapparition de la poudre). Cette phase intermédiaire peut contribuer de manière avantageuse, à améliorer l'homogénéisation du mélange.According to this first variant, the mixture passes intermediarily through a pasty state. In fact, during this operation, there is a step of dissolving the salt (pasty medium) then hydration of the salt (reappearance of the powder). This intermediate phase can advantageously contribute to improving the homogenization of the mixture.
L'opération d'addition de l'eau, en quantité nécessaire et suffisante pour hydrater totalement le sel minéral, a lieu de préférence dans un mélangeur cisaillant, comme notamment les turbosphères, broyeur Henry, mélangeur Stephan, mélangeur Lôdige.The operation of adding water, in an amount necessary and sufficient to completely hydrate the mineral salt, preferably takes place in a shearing mixer, such as in particular the turbospheres, Henry crusher, Stephan mixer, Lodige mixer.
L'addition d'eau peut être progressive ou non.The addition of water may or may not be gradual.
Notons qu'il est préférable de prévoir d'utiliser un appareillage capable d'évacuer les calories dégagées par l'hydratation.Note that it is preferable to plan to use an apparatus capable of evacuating the calories released by hydration.
L'étape de granulation est réalisée de manière classique (pan-granulation, extrusion). Ainsi, le mélange sous forme de particules est mis en contact avec de l'eau de granulation.The granulation step is carried out in a conventional manner (pan-granulation, extrusion). Thus, the mixture in the form of particles is brought into contact with granulation water.
On effectue de préférence l'étape de granulation en présence d'une quantité d'eau permettant d'obtenir un mélange présentant une viscosité appropriée à la mise en forme. Cette teneur en eau dépend bien évidemment de la nature du ou des sels minéraux choisis et de la nature du matériel employé. Elle peut être déterminée sans difficulté par l'homme de l'art. Cependant, à titre d'exemple, la quantité d'eau de granulation varie entre 10 et 20 % en poids par rapport au poids de la composition pour une granulation par agglomération. La granulation a lieu dans tout type d'appareillage approprié.The granulation step is preferably carried out in the presence of an amount of water which makes it possible to obtain a mixture having a viscosity suitable for shaping. This water content obviously depends on the nature of the mineral salt (s) chosen and on the nature of the material used. It can be determined without difficulty by those skilled in the art. However, by way of example, the amount of granulation water varies between 10 and 20% by weight relative to the weight of the composition for granulation by agglomeration. Granulation takes place in any suitable type of apparatus.
Il est à noter que l'on ne sortirait pas du cadre de la présente invention, en ajoutant une quantité d'eau plus importante, puis en mettant en forme le produit par extrusion, avant de le sécher.It should be noted that it would not be departing from the scope of the present invention, by adding a greater quantity of water, then by shaping the product by extrusion, before drying it.
Selon une deuxième variante de préparation du mélange destiné à être séché consiste à granuler au moins un sel minéral sous forme substantiellement hydratée, en présence d'au moins un liant, éventuellement d'au moins un tensioactif, éventuellement d'au moins une charge, et d'eau de granulation.According to a second variant of preparation of the mixture intended to be dried consists in granulating at least one mineral salt in substantially hydrated form, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, and granulation water.
Substantiellement hydraté signifie que le degré d'hydratation du sel minéral est supérieur ou égal à 80 %. La granulation a lieu de manière classique (pan-granulation, extrusion).Substantially hydrated means that the degree of hydration of the mineral salt is greater than or equal to 80%. Granulation takes place in a conventional manner (pan-granulation, extrusion).
Elle peut notamment avoir lieu dans un broyeur/mélangeur ou dans tout type d'appareil permettant d'obtenir un mélange homogène, et plus particulièrement un mélange de poudre homogène. La teneur en eau de granulation mise en œuvre (excepté l'eau de cristallisation, le cas échéant) est de préférence telle que l'on obtienne un mélange présentant une viscosité appropriée à la mise en forme. Cette teneur en eau dépend bien évidemment de la nature du ou des sels minéraux choisis, du matériel utilisé et peut être aisément déterminée par l'homme de l'art. A titre illustratif, la quantité d'eau de granulation (or eau de cristallisation) varie entre 10 et 20 % en poids par rapport au poids de la composition pour une granulation par agglomération.It can in particular take place in a grinder / mixer or in any type of device making it possible to obtain a homogeneous mixture, and more particularly a homogeneous powder mixture. The content of granulation water used (except water of crystallization, if applicable) is preferably such that a mixture is obtained having a viscosity suitable for shaping. This water content obviously depends on the nature of the mineral salt (s) chosen, the material used and can be easily determined by those skilled in the art. By way of illustration, the amount of granulation water (or water of crystallization) varies between 10 and 20% by weight relative to the weight of the composition for granulation by agglomeration.
Un mode de réalisation avantageux de cette variante consiste à apporter le liant avec l'eau de granulation. II est à noter que l'on ne sortirait pas du cadre de la présente invention, en ajoutant une quantité d'eau plus importante, puis en mettant en forme le produit par extrusion, avant de le sécher.An advantageous embodiment of this variant consists in supplying the binder with the granulation water. It should be noted that it would not be departing from the scope of the present invention, by adding a larger quantity of water, then by shaping the product by extrusion, before drying it.
La troisième variante de préparation du mélange destiné à être séché consiste à effectuer les étapes suivantes : . on mélange au moins un sel minéral, en présence d'au moins un liant, éventuellement d'au moins un tensioactif, éventuellement d'au moins une charge, avec la quantité d'eau nécessaire pour obtenir une solution et/ou une dispersion, • on sèche la solution et/ou la dispersion, . on effectue une granulation du mélange séché résultant. Le sel mis en œuvre peut être sous forme anhydre ou hydratée, partiellement ou totalement.The third variant of preparation of the mixture intended to be dried consists in carrying out the following steps:. at least one mineral salt is mixed, in the presence of at least one binder, optionally of at least one surfactant, optionally of at least one filler, with the quantity of water necessary to obtain a solution and / or a dispersion, • the solution and / or the dispersion are dried,. granulation of the resulting dried mixture is carried out. The salt used can be in anhydrous or hydrated form, partially or completely.
Selon cette variante, on passe donc par un état solubilisé et/ou dispersé du ou des éléments constitutifs de la composition. Il est fait remarquer que la composition selon invention étant substantiellement hydrosoluble, on obtient donc substantiellement, au sens de la présente invention, une solution.According to this variant, one therefore goes through a solubilized and / or dispersed state of the constituent element or elements of the composition. It is pointed out that the composition according to the invention being substantially water-soluble, a solution is therefore obtained substantially, within the meaning of the present invention.
La teneur en eau ajoutée peut varier dans de larges limites dès l'instant où un mélange sous forme de solution et/ou de dispersion est obtenu. A titre d'exemple, la teneur en eau ajoutée (or eau de cristallisation) est comprise entre 20 et 60 % en poids d'eau par rapport au poids de la composition sous forme sèche. Une fois la solution/dispersion obtenue, on procède à un séchage de cette dernière. Ce séchage n'a pas pour objectif d'éliminer l'eau de cristallisation, mais l'eau apportée pour l'obtention de la solution/dispersion.The added water content can vary within wide limits from the moment a mixture in the form of solution and / or dispersion is obtained. By way of example, the content of added water (or water of crystallization) is between 20 and 60% by weight of water relative to the weight of the composition in dry form. Once the solution / dispersion has been obtained, the latter is dried. The aim of this drying is not to remove the water of crystallization, but the water supplied to obtain the solution / dispersion.
Cette étape de séchage peut avoir lieu en mettant en œuvre les techniques connues. De manière avantageuse, on effectue le séchage au moyen d'atomiseurs dans lesquels on effectue une pulvérisation du mélange dans une atmosphère chaude (spray- drying). L'atomisation peut être réalisée au moyen de tout pulvérisateur connu en soi, par exemple par une buse de pulvérisation du type pomme d'arrosoir ou autre. On peut également utiliser des atomiseurs dits à turbine. Sur les diverses techniques de pulvérisation susceptibles d'être mises en œuvre dans le présent procédé, on pourra se référer notamment à l'ouvrage de base de MASTERS intitulé "SPRAY-DRYING" (deuxième édition, 1976, Editions George Godwin - London). On notera que l'on peut également réaliser l'opération d'atomisation-séchage au moyen d'un réacteur "flash", par exemple du type décrit notamment dans les demandes de brevet français n° 2 257 326, 2 419 754 et 2 431 321. Dans ce cas, les gaz traitants (gaz chauds) sont animés d'un mouvement hélicoïdal et s'écoulent dans un puits- tourbillon. Le mélange à sécher est injecté suivant une trajectoire confondue avec l'axe de symétrie des trajectoires hélicoïdales desdits gaz, ce qui permet de transférer parfaitement la quantité de mouvement des gaz au mélange à traiter. Les gaz assurent ainsi en fait une double fonction : d'une part la pulvérisation, c'est à dire la transformation en fines particules, du mélange initial, et d'autre part le séchage des fines particules obtenues. Par ailleurs, le temps de séjour extrêmement faible (généralement inférieur à 1/10 de seconde environ) des particules dans le réacteur présente pour avantage, entre autres, de limiter d'éventuels risques de surchauffe par suite d'un contact trop long avec les gaz chauds. En ce qui concerne le réacteur flash précité, on pourra notamment se référer à la figure 1 de la demande de brevet français 2 431 321. La température de ce séchage est telle qu'elle ne dégrade pas les éléments constitutifs de la composition.This drying step can take place using known techniques. Advantageously, the drying is carried out by means of atomizers in which a spraying of the mixture is carried out in a hot atmosphere (spray-drying). The atomization can be carried out by means of any sprayer known per se, for example by a spray nozzle of the sprinkler apple type or the like. We can also use so-called turbine atomizers. On the various spraying techniques likely to be used in the present process, reference may be made in particular to the basic work by MASTERS entitled "SPRAY-DRYING" (second edition, 1976, Editions George Godwin - London). It will be noted that the spray-drying operation can also be carried out by means of a "flash" reactor, for example of the type described in particular in French patent applications 2 257 326, 2 419 754 and 2 431 321. In this case, the treating gases (hot gases) are driven in a helical movement and flow in a vortex well. The mixture to be dried is injected along a trajectory coincident with the axis of symmetry of the helical trajectories of said gases, which allows the momentum of the gases to be transferred perfectly to the mixture to be treated. The gases thus in fact perform a double function: on the one hand the spraying, that is to say the transformation into fine particles, of the initial mixture, and on the other hand the drying of the fine particles obtained. Furthermore, the extremely short residence time (generally less than about 1/10 of a second) of the particles in the reactor has the advantage, inter alia, of limiting possible risks of overheating as a result of too long contact with the hot gases. As regards the above-mentioned flash reactor, reference may in particular be made to FIG. 1 of French patent application 2,431,321. The temperature of this drying is such that it does not degrade the constituent elements of the composition.
On obtient, à l'issue de ce séchage, des particules solides que l'on granule. L'étape de granulation est réalisée de manière classique (pan-granulation, extrusion), en mettant en contact le mélange, sous forme de particules, avec de l'eau de granulation.At the end of this drying, solid particles are obtained which are granulated. The granulation step is carried out in a conventional manner (pan-granulation, extrusion), by bringing the mixture, in the form of particles, into contact with granulation water.
Ce qui a été dit à propos de cette étape pour les variantes précédentes, s'applique à celle-ci. Il suffira donc de s'y reporter.What has been said about this step for the previous variants applies to this one. It will therefore suffice to refer to it.
Il est à noter que l'on peut envisager de mettre en forme le produit en effectuant une granulation par atomisation. Dans ce cas, il est plus approprié de mettre en œuvre cette troisième variante, la granulation étant réalisée simultanément avec l'atomisation. Notons de même, que l'étape de séchage (en d'autres termes, l'élimination des molécules d'eau de cristallisation du sel minéral), peut se faire simultanément dans l'atomiseur.It should be noted that it is possible to envisage shaping the product by carrying out a spray granulation. In this case, it is more appropriate to implement this third variant, the granulation being carried out simultaneously with the atomization. Note also that the drying step (in other words, the elimination of the water molecules of crystallization from the mineral salt), can be done simultaneously in the atomizer.
Si cela est nécessaire, il peut être avantageux de procéder à un tamisage de la composition obtenue après séchage, pour obtenir la granulométrie souhaitée.If necessary, it may be advantageous to screen the composition obtained after drying to obtain the desired particle size.
Un autre objet de la présente invention est donc constitué par une formulation comprenant au moins une matière active absorbée sur la composition selon l'invention. Tout ce qui vient d'être décrit à propos de la composition selon l'invention, de même que de sa préparation reste valable et ne sera donc pas repris ici.Another object of the present invention therefore consists of a formulation comprising at least one active material absorbed on the composition according to the invention. Everything that has just been described about the composition according to the invention, as well as its preparation remains valid and will therefore not be repeated here.
Toutes les matières actives conviennent dans la mesure où elles sont sous forme anhydre ou comprennent une quantité d'eau insuffisante pour solubiliser la composition selon invention.All the active ingredients are suitable insofar as they are in anhydrous form or include an amount of water insufficient to dissolve the composition according to the invention.
Les matières actives peuvent être sous forme liquide à la température de mise en forme ou d'utilisation, dans la mesure où la température de fusion de la matière active reste inférieure à celle de la composition ; sous forme dispersée/solubilisée dans un dispersant/solvant approprié. Ces matières actives peuvent aussi être formulées. Ainsi, elles peuvent être combinées avec d'autres composés comme des tensioactifs, des charges, des additifs classiques dans le domaine en question (anti-mousse, etc.).The active ingredients can be in liquid form at the forming or use temperature, insofar as the melting temperature of the active ingredient remains lower than that of the composition; in dispersed / dissolved form in a suitable dispersant / solvent. These active ingredients can also be formulated. Thus, they can be combined with other compounds such as surfactants, fillers, conventional additives in the field in question (anti-foam, etc.).
Plus particulièrement, ladite formulation peut comprendre au moins une matière active utilisable dans les domaines de la détergence, la cosmétique, l'alimentaire, le phytosanitaire ou le domaine des matériaux de construction.More particularly, said formulation can comprise at least one active material usable in the fields of detergency, cosmetics, food, phytosanitary or the field of building materials.
Les tensioactifs présentant ces caractéristiques, et choisis, par exemple dans ceux listés auparavant, peuvent être mis en œuvre en tant que matière active, utilisables notamment dans les domaines de la détergence, de la cosmétique, etc.The surfactants having these characteristics, and chosen, for example from those listed above, can be used as active material, usable in particular in the fields of detergency, cosmetics, etc.
De préférence, il s'agit de tensioactifs non ioniques. On peut de même citer les substances silicones, sous forme d'huiles, d'émulsions ou de compounds, ainsi que les parfums, les colorants.Preferably, they are nonionic surfactants. Mention may likewise be made of silicone substances, in the form of oils, emulsions or compounds, as well as perfumes, dyes.
Selon une autre possibilité, la formulation peut comprendre au moins une matière active utilisable dans le domaine alimentaire.According to another possibility, the formulation can comprise at least one active material which can be used in the food sector.
Parmi les matières actives convenables, on peut citer les arômes, les huiles essentielles, les vitamines (comme par exemples les vitamines A ou E), les colorants, les composés évitant la formation de mousses, comme les huiles polyéthoxylées dérivées de l'huile de palme, de l'huile de soja, de l'huile de ricin, de l'huile de colza, de l'huile de maïs, de l'huile de tournesol.Among the suitable active ingredients, there may be mentioned flavorings, essential oils, vitamins (such as vitamins A or E), colorants, compounds preventing the formation of foams, such as polyethoxylated oils derived from palm, soybean oil, castor oil, rapeseed oil, corn oil, sunflower oil.
On peut de même citer les agents émulsifiants, stabilisants, épaississants et/ou gélifiants, choisis parmi les esters de sorbitan dérivés d'acides gras alimentaires en Cβ- C22, de préférence en C-10-C20. contenant de 0 à 30 motifs oxyéthylène. A titre d'exemple de tels composés, conviennent le monolauratè de sorbitane, le monooléate de sorbitane, le monopalmitate de sorbitane, le monostéarate de sorbitane, le tristéarate de sorbitane, le monolaurante de polyoxyéthylène sorbitane (20 OE), le monooléate de polyoxyéthylène sorbitane (20 OE), le monopalmitate de polyoxyéthylène sorbitane (20 OE), le monostéarate de polyoxyéthylène sorbitane (20 OE), le tristéarate de polyoxyéthylène sorbitane (20 OE). Peuvent de même être utilisés les sels de sodium, potassium, calcium, d'acides gras alimentaires seuls ou en mélanges, obtenus à partir de matières grasses comestibles, ou d'acides gras alimentaires distillés, les mono- et di-glycérides d'acides gras alimentaires, les mono- et di-glycérides d'acides gras alimentaires estérifiés par des acides carboxyliques tels que les acides acétique, lactique, citrique, tartrique, monoacétyltartrique, diacétyltartrique. Conviennent aussi les sucroesters (esters d'acides gras alimentaires et de saccharose),ainsi que les sucroglycérides qui sont des produits obtenus par transestérification des triglycérides de synthèse ou de préférence naturels par le saccharose. Parmi les sucroglycérides, on peut citer notamment ceux provenant de l'huile de palme, du saindoux, de l'huile de coprah, du suif, de l'huile de colza ou de l'huile de ricin. Un mode opératoire de préparation des sucroglycérides est décrit dans la demande de brevet français FR 2 463 512. Les esters polyglycérides d'acides gras alimentaires ; les esters de polypropylène glycol et d'acides gras alimentaires (monoesters ou en mélange avec des diesters) ; le ricinoléate de polyethylene glycol ; les esters de polyethylene glycol et d'acides gras dérivés d'huiles, comme l'huile de soja ; les esters de glycerol et polyethylene glycol d'acides gras, comme les acides gras du suif ; les éthers de polyglycérol et d'alcools obtenus par réduction des acides oléique et palmitique ; les esters partiels de polyglycérol acides 'gras de ricin polycondensés. Peuvent être mis en oeuvre de manière avantageuse, les polysorbates.Mention may likewise be made of emulsifying, stabilizing, thickening and / or gelling agents, chosen from sorbitan esters derived from dietary fatty acids of Cβ-C22, preferably of C-10-C20. cont oming from 0 to 30 oxyethylene units. Examples of such compounds are sorbitan monolaurate, sorbitan monooleate, sorbitan monopalmitate, sorbitan monostearate, sorbitan tristearate, polyoxyethylene sorbitan (20 EO) monolaurant, polyoxyethylene sorbit monooleate (20 EO), polyoxyethylene sorbitan monopalmitate (20 EO), polyoxyethylene sorbitan monostearate (20 EO), polyoxyethylene sorbitan tristearate (20 EO). Can also be used sodium, potassium, calcium, fatty acids alone or in combination mixtures, obtained from edible fats, or from distilled edible fatty acids, the mono- and di-glycerides of edible fatty acids, the mono- and di-glycerides of edible fatty acids esterified by carboxylic acids such as acetic, lactic, citric, tartaric, monoacetyltartaric, diacetyltartaric acids. Also suitable are sucroesters (esters of fatty acids and sucrose), as well as sucroglycerides which are products obtained by transesterification of synthetic triglycerides or preferably natural by sucrose. Among the sucroglycerides, mention may in particular be made of palm oil, lard, coconut oil, tallow, rapeseed oil or castor oil. A procedure for the preparation of sucroglycerides is described in French patent application FR 2 463 512. Polyglyceride esters of edible fatty acids; esters of polypropylene glycol and edible fatty acids (monoesters or in mixture with diesters); polyethylene glycol ricinoleate; esters of polyethylene glycol and fatty acids derived from oils, such as soybean oil; glycerol and polyethylene glycol esters of fatty acids, such as tallow fatty acids; ethers of polyglycerol and alcohols obtained by reduction of oleic and palmitic acids; polycondensed partial castor fatty acid polyglycerol esters. Polysorbates can be advantageously used.
Selon une autre possibilité, la formulation peut comprendre au moins une matière active utilisable dans le domaine pharmaceutique, les virus, les enzymes.According to another possibility, the formulation can comprise at least one active material usable in the pharmaceutical field, viruses, enzymes.
La formulation comprenant la matière active peut être obtenue en mettant en effectuant une pulvérisation ou une imprégnation de ladite matière active, éventuellement en présence d'un dispersant/solvant, sur la composition selon l'invention. II est à noter, et cela représente un avantage supplémentaire de la composition selon l'invention, que cette étape d'absorption peut être réalisée directement après la préparation de la composition, ou après stockage de la composition.The formulation comprising the active material can be obtained by spraying or impregnating said active material, optionally in the presence of a dispersant / solvent, on the composition according to the invention. It should be noted, and this represents an additional advantage of the composition according to the invention, that this absorption step can be carried out directly after the preparation of the composition, or after storage of the composition.
L'absorption est donc effectuée, de manière classique, par pulvérisation, aspersion ou imprégnation de la matière active sur la composition selon l'invention. La matière active se présente sous la forme d'un liquide, sous forme solubilisée, sous forme fondue.The absorption is therefore carried out, in a conventional manner, by spraying, spraying or impregnating the active material on the composition according to the invention. The active ingredient is in the form of a liquid, in dissolved form, in molten form.
Si l'opération a eu lieu en présence d'un solvant, on effectue ensuite une étape de séchage du granulé résultant.If the operation took place in the presence of a solvent, a step of drying the resulting granule is then carried out.
Il est à noter que l'on ne sortirait pas du cadre de la présente invention en utilisant une formulation selon l'invention, c'est-à-dire comprenant la composition et au moins une matière active, en tant qu'additif (adjuvant) à une formulation plus complexe.It should be noted that it would not be departing from the scope of the present invention to use a formulation according to the invention, that is to say comprising the composition and at least one active material, as an additive (adjuvant ) to a more complex formulation.
Dans ce cas, il suffit de mélanger, durant la préparation même de la formulation complexe, en mettant en œuvre des moyens classiques, la formulation selon l'invention (comprenant la composition et au moins une matière active) avec les autres éléments constitutifs de la formulation plus complexe.In this case, it suffices to mix, during the very preparation of the complex formulation, using conventional means, the formulation according to the invention (comprising the composition and at least one active ingredient) with the other constituent elements of the more complex formulation.
On pourrait de même procéder en préparant séparément la formulation selon l'invention (comprenant la composition et au moins une matière active) avec les autres éléments constitutifs de la formulation complexe pour les mélanger au moment de leur utilisation.One could likewise proceed by preparing the formulation according to the invention separately (comprising the composition and at least one active material) with the other constituent elements of the complex formulation to mix them at the time of their use.
Un exemple concret mais non limitatif de l'invention va maintenant être présenté :A concrete but nonlimiting example of the invention will now be presented:
EXEMPLEEXAMPLE
1 ) Préparation de la composition Dans un broyeur Stephan, on introduit :1) Preparation of the composition In a Stephan mill, the following are introduced:
900 g de Na3PÛ4 anhydre (pyrophosphate) 100 g de Geropon® TA 72 1200 g d'eau (glace).900 g of anhydrous Na3PO4 (pyrophosphate) 100 g of Geropon® TA 72 1200 g of water (ice).
On broie le mélange pendant la durée nécessaire pour obtenir une poudre.The mixture is ground for the time necessary to obtain a powder.
On effectue ensuite une granulation de la poudre en ajoutant 200 g d'eau.Granulation of the powder is then carried out by adding 200 g of water.
Les granulés sont séchés dans un lit fluidisé à 1 10°C pendant une heure puis en étuve, à la même température, pendant 2 heures.The granules are dried in a fluidized bed at 110 ° C. for one hour and then in an oven, at the same temperature, for 2 hours.
A l'issue du séchage, les granulés ont perdu 6,3 % de leur poids.After drying, the granules lost 6.3% of their weight.
2) Absorption d'une matière active2) Absorption of an active ingredient
14,4 g de granulés obtenus précédemment (taille inférieure à 400 μm après tamisage) sont mélangés à 9,6 g d'une composition silicone Rhodorsil® 454 (Rhodia), pendant 10 minutes.14.4 g of granules obtained previously (size less than 400 μm after sieving) are mixed with 9.6 g of a Rhodorsil® 454 silicone composition (Rhodia), for 10 minutes.
On obtient une poudre sèche, indiquant une bonne imprégnation des granulés.A dry powder is obtained, indicating good impregnation of the granules.
La teneur en matière active est de 40 % par rapport au poids total du granulés. The active material content is 40% relative to the total weight of the granules.

Claims

REVENDICATIONS
1. Composition, sous forme de particules solides, substantiellement ou totalement hydrosoluble, dont la capacité d'absorption d'au moins une matière active peut atteindre1. Composition, in the form of solid particles, substantially or completely water-soluble, the absorption capacity of at least one active ingredient of which can reach
50 % en poids, correspondant au rapport en poids de la matière active à la somme de la composition et de la matière active ; ladite composition étant susceptible d'être obtenue à partir d'au moins un sel minéral cristallisant avec au moins une molécule d'eau, d'au moins un liant organique polymérique dont la teneur est inférieure à 30 % en poids de la composition, éventuellement au moins un tensioactif, éventuellement au moins une charge, ladite composition étant susceptible d'être obtenue par un séchage éliminant au moins une partie de l'eau de cristallisation.50% by weight, corresponding to the weight ratio of the active material to the sum of the composition and the active material; said composition being capable of being obtained from at least one mineral salt crystallizing with at least one molecule of water, from at least one polymeric organic binder whose content is less than 30% by weight of the composition, optionally at least one surfactant, optionally at least one filler, said composition being capable of being obtained by drying eliminating at least part of the water of crystallization.
2. Composition selon la revendication précédente, caractérisée en ce que le sel minéral est choisi parmi les phosphates de métal alcalin, le carbonate de métal alcalin, le sulfate de métal alcalin ou d'aluminium, le borate de métal alcalin, les sels d'aluminium, le chlorure de magnésium, ou leurs mélanges.2. Composition according to the preceding claim, characterized in that the mineral salt is chosen from alkali metal phosphates, alkali metal carbonate, alkali metal or aluminum sulfate, alkali metal borate, the salts of aluminum, magnesium chloride, or mixtures thereof.
3. Composition selon la revendication précédente, caractérisée en ce que les phosphates de métal alcalin sont choisis parmi les pyrophosphate, tripolyphosphate, phosphate mono-, di- ou tri-sodique, hexamétaphosphate, ou leurs mélanges.3. Composition according to the preceding claim, characterized in that the alkali metal phosphates are chosen from pyrophosphate, tripolyphosphate, mono-, di- or tri-sodium phosphate, hexametaphosphate, or mixtures thereof.
4. Composition selon l'une quelconque des revendications précédentes, caractérisée en ce que le liant est choisi parmi les monosaccharides, les oligosaccharides, les polymères naturels du type des polysaccharides d'origine animale, végétale, bactérienne, les polymères synthétiques du type des polyalkyleneglycols, de l'alcool polyvinylique, des polymères d'acide (méth)acrylique ou copolymère d'acide (méth)acrylique et de diisobutylène, des acides polyacryliques et leurs sels, des copolymères d'anhydride (ou acide) maleique et d'isobutylene ou de diisobutylène, et leurs sels ; ainsi que leurs mélanges.4. Composition according to any one of the preceding claims, characterized in that the binder is chosen from monosaccharides, oligosaccharides, natural polymers of the type of polysaccharides of animal, plant, bacterial origin, synthetic polymers of the type of polyalkyleneglycols , polyvinyl alcohol, polymers of (meth) acrylic acid or copolymer of (meth) acrylic acid and diisobutylene, polyacrylic acids and their salts, copolymers of maleic anhydride (or acid) and isobutylene or diisobutylene, and their salts; as well as their mixtures.
5. Composition selon l'une quelconque des revendications précédentes, caractérisée en ce qu'elle comprend au moins un tensioactif.5. Composition according to any one of the preceding claims, characterized in that it comprises at least one surfactant.
6. Composition selon l'une quelconque des revendications précédentes, caractérisée en ce qu'elle comprend au moins une charge. 6. Composition according to any one of the preceding claims, characterized in that it comprises at least one filler.
7. Composition selon la revendication précédente, caractérisée en ce que la charge est choisie parmi les terres de diatomées, les argiles comme la bentonite, le kaolin, l'attapulgite, les zéolithes, le carbonate de calcium, le talc, le mica, les silices précipitées, les silicates de métaux alcalins ou alcalino-terreux, la perlite, le charbon, la lignite.7. Composition according to the preceding claim, characterized in that the filler is chosen from diatomaceous earths, clays such as bentonite, kaolin, attapulgite, zeolites, calcium carbonate, talc, mica, precipitated silicas, silicates of alkali or alkaline earth metals, perlite, coal, lignite.
8. Composition selon l'une quelconque des revendications précédentes, caractérisée en ce que le sel minéral précité représente 50 % à moins de 100 % en poids de la composition, plus particulièrement entre 70 et moins de 100 % en poids par rapport à la même référence, de préférence entre 85 et moins de 100 % en poids par rapport à la même référence.8. Composition according to any one of the preceding claims, characterized in that the aforementioned mineral salt represents 50% to less than 100% by weight of the composition, more particularly between 70 and less than 100% by weight relative to the same reference, preferably between 85 and less than 100% by weight relative to the same reference.
9. Composition selon l'une quelconque des revendications précédentes caractérisée en ce que le liant représente entre 0 exclu et 15 % en poids de la composition.9. Composition according to any one of the preceding claims, characterized in that the binder represents between 0 excluded and 15% by weight of the composition.
10. Composition selon l'une quelconque des revendications précédentes caractérisée en ce que le rapport pondéral entre le sel minéral et le liant est compris entre 99,5/0,5 et 60/40, plus particulièrement entre 99,5/05 et 70/30 et de préférence entre 99,5/0,5 et 85/15.10. Composition according to any one of the preceding claims, characterized in that the weight ratio between the mineral salt and the binder is between 99.5 / 0.5 and 60/40, more particularly between 99.5 / 05 and 70 / 30 and preferably between 99.5 / 0.5 and 85/15.
11. Composition selon l'une quelconque des revendications précédentes caractérisée en ce que le tensioactif représente 0 à 15 % en poids de la composition.11. Composition according to any one of the preceding claims, characterized in that the surfactant represents 0 to 15% by weight of the composition.
12. Composition selon l'une quelconque des revendications précédentes caractérisée en ce que la quantité de charge est telle que la composition reste substantiellement ou totalement hydrosoluble.12. Composition according to any one of the preceding claims, characterized in that the amount of filler is such that the composition remains substantially or completely water-soluble.
13. Composition selon la revendication précédente, caractérisée en ce que la quantité de charge est comprise entre 0 et 50 % en poids de la composition.13. Composition according to the preceding claim, characterized in that the amount of filler is between 0 and 50% by weight of the composition.
14. Procédé de préparation de la composition selon l'une quelconque des revendications précédentes, caractérisé en ce que l'on élimine partiellement ou totalement, au moins l'eau de cristallisation, présente dans un mélange comprenant au moins un sel minéral précité, au moins un liant organique polymérique, éventuellement au moins un tensioactif, éventuellement au moins une charge, et de l'eau qui se trouve au moins sous la forme d'eau de cristallisation. 14. Process for preparing the composition according to any one of the preceding claims, characterized in that at least partially or completely, at least the water of crystallization, present in a mixture comprising at least one aforementioned mineral salt, is eliminated, at least one organic polymeric binder, optionally at least one surfactant, optionally at least one filler, and water which is at least in the form of water of crystallization.
15. Procédé de préparation selon la revendication précédente, caractérisé en ce que l'on effectue le séchage d'un mélange obtenu de la manière suivante :15. Preparation process according to the preceding claim, characterized in that the drying of a mixture obtained is carried out as follows:
• on mélange au moins un sel minéral sous forme anhydre ou partiellement hydratée, au moins un liant, éventuellement un tensioactif, éventuellement une charge, avec la quantité d'eau nécessaire et suffisante pour hydrater totalement ledit sel minéral, . on effectue une granulation du mélange résultant.• mixing at least one mineral salt in anhydrous or partially hydrated form, at least one binder, optionally a surfactant, optionally a filler, with the quantity of water necessary and sufficient to completely hydrate said mineral salt,. granulation of the resulting mixture is carried out.
16. Procédé de préparation selon la revendication 14, caractérisé en ce que l'on effectue le séchage d'un mélange obtenu en granulant au moins un sel minéral sous forme substantiellement hydratée, au moins un liant, éventuellement au moins un tensioactif, éventuellement au moins une charge, et de l'eau de granulation.16. Preparation process according to claim 14, characterized in that the drying is carried out of a mixture obtained by granulating at least one mineral salt in substantially hydrated form, at least one binder, optionally at least one surfactant, optionally at minus a filler, and granulation water.
17. Procédé de préparation selon la revendication 14, caractérisé en ce que l'on effectue les étapes suivantes :17. Preparation process according to claim 14, characterized in that the following steps are carried out:
• on mélange au moins un sel minéral, au moins un liant, éventuellement un tensioactif, éventuellement une charge, avec la quantité d'eau nécessaire pour obtenir une solution et/ou une dispersion,At least one mineral salt, at least one binder, optionally a surfactant, optionally a filler, is mixed with the amount of water necessary to obtain a solution and / or a dispersion,
. on sèche la solution et/ou la dispersion, • on effectue une granulation du mélange séché résultant.. the solution and / or the dispersion are dried, • the resulting dried mixture is granulated.
18. Procédé selon l'une quelconque des revendications 14 à 17, caractérisé en ce que l'on effectue l'étape de granulation en présence d'eau.18. Method according to any one of claims 14 to 17, characterized in that the granulation step is carried out in the presence of water.
19. Formulation comprenant au moins une matière active absorbée sur la composition selon l'une quelconque des revendications 1 à 13 ou obtenue conformément au procédé selon l'une quelconque des revendications 14 à 18.19. Formulation comprising at least one active material absorbed on the composition according to any one of claims 1 to 13 or obtained according to the process according to any one of claims 14 to 18.
20. Formulation selon l'une des revendications 19, caractérisée en ce qu'elle est utilisable en tant qu'adjuvant.20. Formulation according to one of claims 19, characterized in that it can be used as an adjuvant.
21. Procédé de préparation de la formulation selon l'une quelconque des revendications 19 ou 20, caractérisé en ce que l'on effectue une pulvérisation ou une imprégnation de la matière active, sous la forme d'un liquide, sur la composition selon l'une quelconque des revendications 1 à 13.21. A method of preparing the formulation according to any one of claims 19 or 20, characterized in that a spraying or impregnation of the active material is carried out, in the form of a liquid, on the composition according to l any of claims 1 to 13.
21. Procédé selon la revendication précédente, caractérisé en ce que l'on sèche éventuellement le produit résultant. 21. Method according to the preceding claim, characterized in that the resulting product is optionally dried.
22. Procédé de préparation de la formulation selon la revendication 19, caractérisé en ce que l'on effectue une pulvérisation ou une imprégnation de la matière active, sous la forme d'un liquide, sur la composition selon l'une quelconque des revendications 1 à 12, en ce que l'on sèche éventuellement le produit résultant, et en ce qu'on le mélange aux autres éléments constitutifs de la formulation, durant la préparation de cette dernière ou au moment de son utilisation. 22. Method for preparing the formulation according to claim 19, characterized in that a spraying or impregnation of the active material is carried out, in the form of a liquid, on the composition according to any one of claims 1 to 12, in that the resulting product is optionally dried, and in that it is mixed with the other constituent elements of the formulation, during the preparation of the latter or at the time of its use.
EP00917117A 1999-04-02 2000-04-03 Mineral-salt based substantially or totally hydrosoluble composition, formulation containing said composition and production thereof Withdrawn EP1183100A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9904184 1999-04-02
FR9904184A FR2791581B1 (en) 1999-04-02 1999-04-02 COMPOSITION BASED ON SUBSTANTIALLY OR TOTALLY WATER-SOLUBLE MINERAL SALT, FORMULATION COMPRISING SAME, AND PREPARATIONS THEREOF
PCT/FR2000/000834 WO2000059628A1 (en) 1999-04-02 2000-04-03 Mineral-salt based substantially or totally hydrosoluble composition, formulation containing said composition and production thereof

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EP1183100A1 true EP1183100A1 (en) 2002-03-06

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EP (1) EP1183100A1 (en)
JP (1) JP2002541267A (en)
AU (1) AU3823600A (en)
BR (1) BR0009538A (en)
CA (1) CA2365862A1 (en)
FR (1) FR2791581B1 (en)
WO (1) WO2000059628A1 (en)
ZA (1) ZA200107945B (en)

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JP2002541267A (en) 2002-12-03
AU3823600A (en) 2000-10-23
ZA200107945B (en) 2002-05-08
WO2000059628A1 (en) 2000-10-12
CA2365862A1 (en) 2000-10-12
BR0009538A (en) 2003-03-05
FR2791581A1 (en) 2000-10-06
FR2791581B1 (en) 2001-05-18

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