CA2365862A1 - 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 Download PDFInfo
- Publication number
- CA2365862A1 CA2365862A1 CA002365862A CA2365862A CA2365862A1 CA 2365862 A1 CA2365862 A1 CA 2365862A1 CA 002365862 A CA002365862 A CA 002365862A CA 2365862 A CA2365862 A CA 2365862A CA 2365862 A1 CA2365862 A1 CA 2365862A1
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- Prior art keywords
- composition
- water
- composition according
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- 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.)
- Abandoned
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 174
- 238000009472 formulation Methods 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 150000003839 salts Chemical class 0.000 claims abstract description 58
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 39
- 239000011707 mineral Substances 0.000 claims abstract description 39
- 239000011230 binding agent Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 230000008025 crystallization Effects 0.000 claims abstract description 21
- 238000010521 absorption reaction Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 14
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000004480 active ingredient Substances 0.000 claims description 30
- 238000005469 granulation Methods 0.000 claims description 25
- 239000004094 surface-active agent Substances 0.000 claims description 24
- 230000003179 granulation Effects 0.000 claims description 22
- -1 alkali metal borate Chemical class 0.000 claims description 16
- 239000000945 filler Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- 239000011149 active material Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 6
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 150000004676 glycans Chemical class 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 229910000318 alkali metal phosphate Inorganic materials 0.000 claims description 3
- 230000001580 bacterial effect Effects 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 3
- 235000011180 diphosphates Nutrition 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
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- 239000005017 polysaccharide Substances 0.000 claims description 3
- 229920001059 synthetic polymer Polymers 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 3
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 claims description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 2
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229960000892 attapulgite Drugs 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 239000011363 dried mixture Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 229940005740 hexametaphosphate Drugs 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003077 lignite Substances 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 229920005615 natural polymer Polymers 0.000 claims description 2
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- 239000002244 precipitate Substances 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- FXNDIJDIPNCZQJ-UHFFFAOYSA-N 2,4,4-trimethylpent-1-ene Chemical group CC(=C)CC(C)(C)C FXNDIJDIPNCZQJ-UHFFFAOYSA-N 0.000 claims 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims 1
- 238000000889 atomisation Methods 0.000 abstract description 5
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- 239000013543 active substance Substances 0.000 abstract 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
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- 235000014113 dietary fatty acids Nutrition 0.000 description 15
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- 229930195729 fatty acid Natural products 0.000 description 15
- 150000004665 fatty acids Chemical class 0.000 description 15
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- 150000002148 esters Chemical class 0.000 description 6
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- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 4
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 4
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
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- 244000303965 Cyamopsis psoralioides Species 0.000 description 2
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- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 1
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- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 1
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- LIKRJSFVBBUVIT-UHFFFAOYSA-M sodium 4-(3-ethyloctan-4-yloxy)-4-oxo-3-sulfobutanoate Chemical compound [Na+].CCCCC(C(CC)CC)OC(=O)C(CC([O-])=O)S(O)(=O)=O LIKRJSFVBBUVIT-UHFFFAOYSA-M 0.000 description 1
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- 159000000000 sodium salts Chemical class 0.000 description 1
- GCNLRNBDDUYJMP-UHFFFAOYSA-M sodium;2-methylnaphthalene-1-sulfonate Chemical compound [Na+].C1=CC=CC2=C(S([O-])(=O)=O)C(C)=CC=C21 GCNLRNBDDUYJMP-UHFFFAOYSA-M 0.000 description 1
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- 239000001589 sorbitan tristearate Substances 0.000 description 1
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- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
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- 150000003626 triacylglycerols Chemical class 0.000 description 1
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- 238000009736 wetting Methods 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
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Classifications
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Abstract
Description
COMPOSITION A BASE D'UN SEL MINERAL SUBSTANTIELLEMENT OU
TOTALEMENT HYDROSOLUBLE, FORMULATION LA COMPRENANT, ET
LEURS 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.
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.
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.
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, plûs 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 détergente, 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.
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.
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 oeuvre un traitement thermique très contrôlé, dont le but est d'éliminer les 10 moles d'eau présentes, créant COMPOSITION BASED ON SUBSTANTIALLY OR MINERAL SALT
TOTALLY WATER SOLUBLE, FORMULATION COMPRISING SAME, AND
THEIR PREPARATIONS
The subject of the present invention is a composition in the form of particles.
solid, substantially or fully water-soluble, comprising a salt mineral crystallizing with at least one molecule of water, a binder. The composition is susceptible to be obtained by a drying operation at least partially eliminating the water of crystallization of said salt.
It also relates to a formulation comprising at least one material active ingredient absorbed on the aforementioned composition, and the process for preparing said formulation.
In many technical fields, attempts have been made to prepare powders flowable based on liquid or solubilized active ingredients. From possibilities include that of forming a grain in which the active material is absorbed.
One of the problems to be resolved relates to the absorption capacity of the grain. In effect, the latter must be as high as possible so as to obtain, after absorption, the highest possible concentration of active ingredient.
Another difficulty, which happens to be the consequence of an ability absorption high, is the grain attrition resistance. Indeed, the greater the capacity absorption is the higher the porosity, the lower the attrition resistance important, which suggests storage difficulties for example, grain alone, but possibly also of the complete formulation.
In the detergent field, preparation processes are known comprising two stages, the first consisting in preparing the grain alone, and the second to spray on the latter, the active material, which happens to be good often a nonionic surfactant.
The grain is obtained by atomization of a mixture comprising in particular a salt of the silicate, phosphate type and, if appropriate, comprising other additives like the anti-redeposition agents. The active ingredient, possibly also additive, is then sprayed on the grains obtained.
If advantages exist with such a process, the fact remains that the absorption capacity of the granule remains somewhat low.
Certainly there are, in the prior art, methods of. preparation of compounds very absorbent, such as sodium carbonate for example. The processes consist, from sodium carbonate decahydrate, to implement a treatment very controlled thermal, the purpose of which is to eliminate the 10 moles of water present, creating
2 de ce fait une porosité importante dans les particules. Cependant, ces dernières ont une taille qui ne dépasse pas 10 Nm 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.
II 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 %.
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.
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.
Un autre objet de l'invention est relatif à une formulation comprenant au moins une matière active absorbée sur la composition selon l'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.
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). 2 therefore a large porosity in the particles. However, these last have a size which does not exceed 10 Nm on average. Therefore, if their capacity absorption is very important, such particles are not always desired, because they require precautions of use because of their character powdery.
The object of the present invention is therefore to propose a composition which may serve as a matrix for an active material intended to be absorbed therein, composition that is totally or substantially water-soluble, very absorbent and not powdery.
It should be noted that by substantially means within the meaning of this invention, that more than 50% of said composition is dissolved in water, more particularly, at least 80%, preferably at least 90%.
Thus, a first object of the invention consists of a composition, under form of solid particles, substantially or completely water-soluble, whose absorption capacity of at least one active ingredient can reach 50% in weight, corresponding to the weight ratio of the active ingredient to the sum of the composition and active ingredient; said composition being capable of being obtained at from at at least one mineral salt crystallizing with at least one molecule of water, at least minus a binder organic polymer whose content is less than 30% by weight of the composition, optionally at least one surfactant, optionally at least one charge, said composition being capable of being obtained by drying eliminating at least a part water of crystallization.
A second subject of the invention relates to a process for the preparation of said composition in which at least the water is partially or totally eliminated of crystallization, present in a mixture comprising at least one mineral salt above, at least one organic polymeric binder, optionally at least one surfactant, possibly at least one charge, and water which is at least under the form water of crystallization.
Another subject of the invention relates to a formulation comprising at least less an active material absorbed on the composition according to the invention.
Finally, a last object of the invention relates to the preparation of said formulation; process in which spraying or impregnation of the active ingredient, in the form of a liquid, on the composition according to the invention.
As has been mentioned before, the composition according to the invention has the advantage of having a very high absorption capacity. Indeed, he 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 presents absorption which can be as high as 50% (weight ratio of matter active to the sum of the composition and the active ingredient).
3 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.
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.
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.
La composition selon l'invention peut être employée pour obtenir des formulations solides alors que la matière active est liquide, fondue ou solubilisée.
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).
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.
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.
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.
Ainsi que cela a été indiqué précédemment, la composition selon l'invention comprend un sel minéral cristallisant avec au moins une molécule d'eau. 3 The absorption capacity is measured relative to Rhodasurf ID 79, which is a nonionic surfactant (isodecyl alcohol comprising 7 oxide units ethylene marketed by Rhodia Chimie). The test is to put the composition in contact with the surfactant, at room temperature, gradually and under agitation, up the mixture takes on a sticky appearance (the solid mixture no longer flows of fluid way - not free-flowing). We then assess the amount of surfactant added.
Due to 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, pharmaceutical industry, agrochemical industry.
Furthermore, the composition according to the invention consists of particles porous not powdery, the size of which is sufficient not to pose problems of handling.
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.
The composition according to the invention can be used to obtain formulations solids while the active ingredient is liquid, molten or dissolved.
The composition according to the invention has the advantage of being able to mix in a same packaging of substances which would have been incompatible in mixture liquid (if the substances are chemically reactive with each other, for example).
In addition, the composition according to the invention can be adapted according to the active ingredients for which it will serve as a support. So the composition according to the invention can advantageously be used for active ingredients sensitive to pH.
Note as an additional advantageous characteristic of the composition according to the invention, that it contributes to facilitating the use of the formulation which contains. Indeed, the composition according to the invention gives said formulation, more or less rapid dissolution properties and above all, adjustable.
The hardness of the granule (resistance to attrition), its absorption capacity, its pH, can also, and this represents interesting features of the composition of the invention, be adjusted according to the subsequent uses of the formulations that understand.
Finally, the process for preparing the composition according to the invention is simple and allows to obtain various forms of particles.
But other characteristics and advantages of the present invention will appear more clearly on reading the description and examples that go to follow.
As indicated above, the composition according to the invention includes a mineral salt crystallizing with at least one molecule of water.
4 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 oeuvre de l'invention les pyrophosphate, tripolyphosphate, phosphate mono-, di- ou tri-sodique, hexamétaphosphate, ou leurs mélanges.
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.
De préférence, les sels minéraux mis en oeuvre pour la préparation de la composition selon l'invention ne comprennent pas de tripolyphosphate seul.
Selon un mode avantageux, les sels mis en oeuvre ne comprennent dè 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.
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 polyalkylèneglycols, de l'alcool polyvinylique, des polymères d'acide (méth)acrylique ou copolymère d'acide (méth)acrylique et d'isobutylène ou de düsobutylène, des acides polyacryliques et leurs sels, des copolymères d'anhydride (ou acide) maléfique et d'isobutylène ou de düsobutylène, 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.
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.
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'isobutylène ou de düsobutylène, ainsi que leurs sels.
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 4 More particularly the mineral salt is chosen from metal phosphates alkali, alkali metal carbonate, alkali metal sulfate or aluminum, the alkali metal borate, aluminum salts, magnesium chloride, or their mixtures.
With particular regard to the alkali metal phosphates, suitable for implementing the invention, pyrophosphate, tripolyphosphate, mono-, di- or tri-sodium phosphate, hexametaphosphate, or mixtures thereof.
Preferably, the composition according to the invention comprises, as salt mineral to minus a salt chosen from phosphates, and in particular those mentioned, as well that carbonates of alkali metal, and more particularly of sodium.
Preferably, the mineral salts used for the preparation of the composition according to the invention do not include tripolyphosphate alone.
According to a advantageous mode, the salts used do not include tripolyphosphate or alone neither 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 salt mineral is between 70 and less than 100% by weight compared to the same reference. Preferably, the amount of mineral salt is between 85 and less of 100% by weight compared to the same reference.
The composition according to the invention also comprises at least one binder organic polymeric.
Among the compounds capable of being used, alone or in combination, in so much as a binder, mention may be made of monosaccharides, oligosaccharides, polymers natural types of polysaccharides of animal, vegetable, bacterial origin, the synthetic polymers such as polyalkylene glycols, alcohol polyvinyl, (meth) acrylic acid polymers or (meth) acrylic acid copolymer and isobutylene or isobutylene, polyacrylic acids and their salts, copolymers of maleic anhydride (or acid) and isobutylene or dobsylene, and their salts, as well as their mixtures.
Lactose, sucrose, alone or as a mixture, represent examples possible binders chosen from monosaccharides and oligosaccharides.
With regard to natural polymers of the polysaccharide type original animal, vegetable, bacterial, there may be mentioned by way of nonlimiting example, gum xanthan, guar and derivatives (such as hydroxypropyl guar for example), polydextroses, or combinations thereof.
Among the synthetic polymers, especially suitable, alone or as a mixture, polyethylene glycols, polypropylene glycols, polybutylene glycols, copolymers of polyethylene- and polypropylene- glycols, polyvinyl alcohol, polymers acid (meth) acrylic or copolymers of (meth) acrylic acid and isobutylene or dobsylene, and their salts.
Also particularly suitable, and this represents an embodiment preferred of the invention, acrylic acid polymers such as Geropon ~
HB, as well
5 que les copolymères d'anhydride (ou d'acide) maléfique et de düsobutylène.
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 C~-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).
La quantité d'agent liant est plus particulièrement comprise entre 0 exclu et 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.
II 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.
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.
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(S03M)-COOR', où R représente un radical alkyle en Cg-C2o, de préférence en Cep-C16, R' un radical alkyle en C~-C6, de préférence en C~-C3 et M un cation alcalin (sodium, potassium, lithium), ammonium substitué ou non substitué (méthyl-, diméthyl-, triméthyl-, tetraméthylammonium, diméthylpiperidinium ...) ou dérivé d'une alcanolamine 5 as the copolymers of maleic anhydride (or acid) and düsobutylène.
These copolymers can be in the acid form or else in a form of alkali metal or ammonium salt of type N (R) 4+, with R, identical or different, representing hydrogen atoms, or C ~ -C4 hydrocarbon radicals.
Of preferably, the copolymer is in the form of the sodium salt.
These copolymers are well known compounds and are in particular sold under the name GEROPON ~ T 36 (Rhodia).
The amount of binding agent is more particularly between 0 excluded and by weight of the composition according to the invention. According to one embodiment particular of the invention, the amount of binder is between 0 excluded and 15% by weight compared to the same reference. However, according to a very preferred variant of the invention, the binder content is between 0.5 and 15% by weight relative to the composition.
It should be noted that if the composition according to the invention only comprises salt mineral and the polymeric binder, the respective contents of these compounds are as the whole represents 100% by weight.
According to one embodiment of the invention, the weight ratio between the salt mineral and the binder is between 99.5 / 0.5 and 60/40. More specifically said report by weight is between 99.5 / 05 and 70/30, preferably between 99.5 / 0.5 and 85/15.
The composition according to the invention can likewise comprise, where appropriate, at minus one surfactant.
Without wishing to be limited by any theory, the surfactant, when East present, has two roles, that of optimizing the wetting of the mineral salt and binder, and that to optimize the dispersion of the active ingredient during its use.
All the surfactants can be suitable for the invention, insofar as they are compatible with the active ingredient Thus, it is possible to use surfactants anionic, nonionic, cationic, zwitterionic or amphoteric.
Among the anionic surfactants that may be mentioned by way of example Polymers derived from lignin such as sodium lignosulfonates or calcium;
alkyl esters sulfonates of formula R-CH (S03M) -COOR ', where R represents a alkyl radical in Cg-C2o, preferably in Cep-C16, R 'an alkyl radical in C ~ -C6, preferably in C ~ -C3 and M an alkaline cation (sodium, potassium, lithium), substituted or unsubstituted ammonium (methyl-, dimethyl-, trimethyl-, tetramethylammonium, dimethylpiperidinium ...) or derived from an alkanolamine
6 (monoéthanolamine, diéthanolamine, triéthanolamine ...). On peut citer tout particulièrement les méthyl ester sulfonates dont le radical R est en C~4-C16 les alkylsulfonates primaires ou secondaires en Cg-C2o ;
les alkylarylsulfonates comme l'isopropylnaphtalène sulfonate de sodium, commercialisé sous le nom Supragil WP~ ; les alkylbenzènesulfonates en Cg-C2o ;
les méthylnaphtalène sulfonate de sodium condensés comme le Supragil MNS90~, les sulfonates de paraffine.
les alkylsulfates de formule ROS03M, où R représente un radical alkyle ou hydroxyalkyle en C~o-C24, de préférence en C~2-C2o et tout particulièrement en C~2-C~g, 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/ou OP;
les sulfates d'alkylglycosides ;
les alkylalryl sulfates, comme les mono-, di- ou tri-tristyryl phénols polyoxyalkylénés (OE et/ou OP); éventuellement neutralisés en totalité ou partiellement ;
les alkylamides sulfates de formule RCONHR'OS03M où R représente un radical alkyle en C2-C22, de préférence en C6-C2o, 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 Cg-C24, de préférence en C~4-C2o les acides polycarboxyliques sulfonés décrits dans GB-A-1 082 179 ;
les polyéthoxycarboxylates, le cation étant de même définition que précédemment , ~ 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 ;
les alkylsuccinamates ;
~ les alkylphosphates Parmi les tensioactifs non-ioniques, on peut mentionner comme exemple les dérivés polyoxyalkylénés d'alcools aliphatiques ou arylaliphatiques en Cg-contenant de 1 à 25 motifs oxyalkylénés (oxyéthyléné, oxypropyléné), les alkylphénols polyoxyalkylénés (polyéthoxyéthylénés, polyoxypropylénés, polyoxybutylénés) dont le substituant alkyle est en C6-C~2 et contenant de 5 à
motifs oxyalkylènes, 6 (monoethanolamine, diethanolamine, triethanolamine ...). We can quote everything particularly methyl ester sulfonates whose radical R is C ~ 4-C16 primary or secondary Cg-C2o alkylsulfonates;
alkylarylsulfonates such as sodium isopropylnaphthalene sulfonate, marketed under the name Supragil WP ~; Cg-C2o alkylbenzenesulfonates ;
condensed sodium methylnaphthalene sulfonate such as Supragil MNS90 ~, paraffin sulfonates.
alkyl sulfates of formula ROS03M, where R represents an alkyl radical or hydroxyalkyl C ~ o-C24, preferably C ~ 2-C2o and especially C ~ 2-C ~ g, M representing a hydrogen atom or a cation of the same definition as above, as well as their ethoxylenated (OE) and / or propoxylenated derivatives (OP), with an average of 0.5 to 6 units, preferably 0.5 to 3 OE units and or OP;
alkyl glycoside sulfates;
alkylalryl sulfates, such as mono-, di- or tri-tristyryl phenols polyoxyalkylenated (OE and / or OP); possibly neutralized in whole or in part;
the alkylamide sulfates of formula RCONHR'OS03M where R represents a radical C2-C22 alkyl, preferably C6-C2o, R 'a C2-C3 alkyl radical, M
representing a hydrogen atom or a cation of the same definition as above above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having in average of 0.5 to 60 OE and / or OP units;
salts of saturated or unsaturated fatty acids with Cg-C24, preferably with C ~ 4-C2o the sulfonated polycarboxylic acids described in GB-A-1 082 179;
polyethoxycarboxylates, the cation being of the same definition as previously, ~ alkylsulfosuccinates, monoesters or diesters of sulfosuccinates, as the sodium di-ethyl-2-hexyl sulfosuccinate, N-acyl sarcosinates, N-acyl N-alkyl taurates;
alkylisethionates;
alkylsuccinamates;
~ alkylphosphates Among the nonionic surfactants, there may be mentioned as an example polyoxyalkylenated derivatives of aliphatic or arylaliphatic alcohols in Cg-containing from 1 to 25 oxyalkylenated (oxyethylenated, oxypropylenated) units, the polyoxyalkylenated alkylphenols (polyethoxyethylenated, polyoxypropylenated, polyoxybutylenated) whose alkyl substituent is C6-C ~ 2 and containing from 5 to oxyalkylene units,
7 les alkylpolysaccharides présentant un groupement hydrophobe en C6-C3o, de préférence en Cep-C~6 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'amines tels que les oxydes d'alkyl Cep-C~$ diméthylamines, les oxydes d'alkoxy Cg-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 Cg-C2p, les acides gras éthoxylés, les amides gras éthoxylés, les amines éthoxylées.
Comme tensioactifs cationiques, on peut citer tout particulièrement les halogénures d'alkyldiméthylammonium.
A titre de tensioactifs amphotères et zwitterioniques, conviennent les alkyldiméthylbétaïnes, les alkylamidopropyldiméthylbétaïnes, les alkyltriméthyl-sulfobétaïnes, les alkylsultaïnes, les alkylamidopropylhydroxysultaïnes, 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, les dérivés d'imidazoline 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.
La composition selon l'invention peut éventuellement comprendre au moins une charge.
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, 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. Ces composés peuvent être présents seuls ou en mélanges.
La quantité de charge est de préférence telle que la composition reste substantiellement ou totalement hydrosoluble.
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 WO 00/59627 alkylpolysaccharides having a hydrophobic group C6-C3o, preferably in Cep-C ~ 6 and a polysaccharide group, for example polyglycoside, as a hydrophilic group as well as from 1 to 3 sugar units, alkylated amino sugar derivatives, such as alkylglucamides produced by the amidification reaction of a fatty acid on N-methylglucamine, oxides amines such as Cep-C ~ $ dimethylamine alkyl oxides, oxides alkoxy Cg-C22 ethyl dihydroxy ethylamines, alkylglucamides, glycerolamides derivatives N-alkylamines (US-A-5,223,179 and FR-A-1,585,966), fatty acid amides in Cg-C2p, ethoxylated fatty acids, fatty amides ethoxylated, ethoxylated amines.
As cationic surfactants, mention may be made most particularly of alkyldimethylammonium halides.
As amphoteric and zwitterionic surfactants, suitable alkyldimethylbetaines, alkylamidopropyldimethylbetaines, alkyltrimethyl-sulfobetaines, alkylsultaines, alkylamidopropylhydroxysultaines, the condensation products of fatty acids on proteins or hydrolysates of protein, amphoteric derivatives of alkylpolyamines such as Amphionic XL ~ sold by Rhodia, Ampholac 7T / X ~ and Ampholac 7C / X ~ marketed by Berol Nobel, imidazoline 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%
in weight relative to the weight of the composition. More specifically, it is understood between 0 and 5% by weight compared to the same reference.
The composition according to the invention can optionally comprise at least one charge.
Among the fillers which can be used in the composition according to the invention, it is possible to to quote for example diatomaceous earth, clays such as bentonite, kaolin, attapulgite, zeolites; calcium carbonate, talc, mica, silicas precipitates, alkali or alkaline earth metal silicates, perlite, coal, lignite. These compounds can be present alone or in mixtures.
The amount of filler is preferably such that the composition remains substantially or completely water-soluble.
More particularly, the amount of filler in the composition represents 0 at 50% by weight relative to the weight of the composition. According to a mode of production particular of the invention, the amount of filler represents 0 to 30% by weight, and WO 00/5962
8 PCT/FR00/00834 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.
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.
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.
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.
II 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 oeuvre dans une étuve, et de préférence en lit fluidisé.
Le séchage, avantageusement, a lieu sous air, à pression atmosphérique ou sous pression réduite.
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.
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.
L'opération de séchage a lieu sur un mélange qui peut être obtenu selon plusieurs variantes avantageuses.
Une première variante consiste à effectuer ledit séchage sur un mélange obtenu de la manière suivante . 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, . on effectue une granulation, plus particulièrement à l'aide d'une solution aqueuse, du mélange résultant. 8 PCT / FR00 / 00834 preferably 0 to 10% by weight relative to the same reference. A mode of production more preferred of the invention is not to use a filler.
The sum of all the above-mentioned compounds (mineral salt, binder, surfactant, charge), represents 100% by weight of the composition.
The process for preparing the composition according to the invention will now to be described in more detail.
As mentioned above, the process for preparing the composition according to the invention, consists in partially eliminating or totally, at least water of crystallization, present in a mixture comprising at least one salt mineral mentioned above, at least one binder, optionally at least one surfactant, possibly at minus a filler, and water which is at least in the form of water from crystallization.
This drying step, during which the water, which is present at least under the form of water of crystallization, is eliminated, allows to adjust the capacity absorption granulated, depending on whether the water of crystallization is more or less removed from the salt mineral.
It should be noted that the drying operation also makes it possible to eliminate all or in part, and preferably all, of the water likely to be provided during of obtaining of the mixture to be dried, in addition to the water of crystallization. The operation of drying will described below.
This drying operation can advantageously be carried out in a 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 constituent compounds composition according to the invention. In addition, it must be high enough for allow a departure of the water of crystallization of the mineral salt.
Without intending to be limited thereto, the temperature range can be understood 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 many advantageous variants.
A first variant consists in carrying out said drying on a mixture obtained as follows . at least one mineral salt is mixed in anhydrous or partially form hydrated, in the presence of at least one binder, optionally at least one surfactant, optionally at least one filler, with the amount of water necessary and sufficient to completely hydrate said mineral salt, . granulation is carried out, more particularly using a solution aqueous, of the resulting mixture.
9 Par partiellement hydraté, on entend désigner un sel minéral dont le taux d'hydratation est inférieur à 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.
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 Lddige.
L'addition d'eau peut étre progressive ou non.
Notons qu'il est préférable de prévoir d'utiliser un appareillage capable d'évacuer les calories dégagées par l'hydratation.
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.
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.
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.
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.
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).
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 ceuvre (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 5 déterminée par l'homme de l'art. A titre illustratif, ta 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.
Un mode de réalisation avantageux de cette variante consiste à apporter le liant avec l'eau de granulation. 9 By partially hydrated is meant a mineral salt whose rate hydration is less than 80%.
According to this first variant, the mixture passes through an intermediate state pasty. Indeed, during this operation, we go through a step of salt dissolution (pasty medium) then by hydration of the salt (reappearance of the powder).
This phase intermediary can make an advantageous contribution to improving homogenization of the mixture.
The operation of adding water, in a quantity necessary and sufficient for hydrate totally the mineral salt, preferably takes place in a shearing mixer, as including turbospheres, Henry crusher, Stephan mixer, mixer Lddige.
The addition of water may or may not be gradual.
Note that it is preferable to plan to use a device capable to evacuate calories released by hydration.
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 some water granulation.
The granulation step is preferably carried out in the presence of a quantity of water making it possible to obtain a mixture having a viscosity suitable for placing in form.
This water content obviously depends on the nature of the salt (s) minerals chosen and the nature of the material used. She may be determined without difficulty by those skilled in the art. However, as an example, the quantity of water granulation 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.
It should be noted that it would not go beyond the scope of the present invention, in adding more water and then shaping the produced by extrusion, before drying.
According to a second variant of preparation of the mixture intended to be dried consists in granulating at least one mineral salt in form substantially hydrated, presence of at least one binder, optionally at least one surfactant, eventually at least one charge, and granulation water.
Substantially hydrated means that the degree of hydration of the mineral salt East greater than or equal to 80%.
Granulation takes place in a conventional manner (pan-granulation, extrusion).
It can in particular take place in a grinder / mixer or in any type apparatus for obtaining a homogeneous mixture, and more particularly a homogeneous powder mixture.
The content of granulation water used (except water from crystallization, the preferably) is preferably such that a mixture having a viscosity suitable for shaping. This water content depends well obviously the nature of the mineral salt (s) chosen, the material used and may be easily 5 determined by those skilled in the art. As an illustration, your amount of water from granulation (gold water of crystallization) varies between 10 and 20% by weight relative to the weight of the composition for agglomeration granulation.
An advantageous embodiment of this variant consists in providing the binder with granulation water.
10 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.
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 oeuvre peut être sous forme anhydre ou hydratée, partiellement ou totalement.
Selon cette variante, on passe donc par un état solubilisé et/ou dispersé du ou des éléments constitutifs de la composition. II est fait remarquer que la composition selon invention étant substantiellement hydrosoluble, on obtient donc substantiellement, au sens de la présente invention, une solution.
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.
Cette étape de séchage peut avoir lieu en mettant en oeuvre 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 WO 00!59628 PCT/FR00/00834 10 It should be noted that it would not go beyond the scope of ~ this invention, in adding more water and then shaping the produced by extrusion, before drying.
The third variant for preparing the mixture intended to be dried consists at perform the following steps . at least one mineral salt is mixed, in the presence of at least one binder, optionally at least one surfactant, optionally at least one charge, 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 totally.
According to this variant, there is therefore a solubilized and / or dispersed state of the or of the constituent elements of the composition. It is pointed out that the composition according to the invention being substantially water-soluble, we therefore obtain substantially, within the meaning of the present invention, a solution.
The added water content can vary within wide limits from the moment that a mixing in the form of a solution and / or dispersion is obtained. As for example, the added water content (or water of crystallization) is between 20 and 60 % in weight of water relative to the weight of the composition in dry form.
Once the solution / dispersion has been obtained, this is dried.
last. This drying is not intended to remove water from crystallization but the water brought to obtain the solution / dispersion.
This drying step can take place using the techniques known.
Advantageously, the drying is carried out by means of atomizers in which are sprayed with the mixture in a hot atmosphere (spray-drying). The atomization can be carried out using any known sprayer in itself, by example by a spray nozzle of the apple type watering can or other. We can WO 00! 59628 PCT / FR00 / 00834
11 également utiliser des atomiseurs dits à turbine. Sur les diverses techniques de pulvérisation susceptibles d'être mises en oeuvre 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'àutre 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.
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.
Ce qui a été dit à propos de cette étape pour les variantes précédentes, s'applique à celle-ci. II suffira donc de s'y reporter.
II 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 oeuvre 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.
Si cela est nécessaire, il peut être avantageux de procéder à un tamisage de la composition obtenue après séchage, pour obtenir la granulométrie souhaitée.
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. 11 also use so-called turbine atomizers. On the various techniques of spray which can be used in the present process, will be able refer in particular to the MASTERS basic work entitled "SPRAY-DRYING"
(second edition, 1976, Editions George Godwin - London).
Note that we can also perform the spray-drying operation at by means of a "flash" reactor, for example of the type described in particular in requests French Patent Nos. 2,257,326, 2,419,754 and 2,431,321. In this case, treating gases (hot gases) are driven in a helical movement and flow into a well-whirlwind. The mixture to be dried is injected along a combined path with the axis of symmetry of the helical trajectories of said gases, which makes it possible to to transfer perfectly the momentum of the gases in the mixture to be treated. Gas ensure thus makes it a double function: on the one hand the spraying, ie the transformation into fine particles, of the initial mixture, and on the other hand the drying fine particles obtained. Furthermore, the extremely short residence time (usually less than about 1/10 of a second) of the particles in the reactor has the advantage, among other things, of limiting possible risks of overheating by following too long contact with hot gases. About the flash reactor cited above, reference may in particular be made to FIG. 1 of the patent application French 2,431,321.
The temperature of this drying is such that it does not degrade the elements of the composition.
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 into contact, in the form of particles, with some water granulation.
What has been said about this step for the previous variants, applies to it. It will therefore suffice to refer to it.
It should be noted that one can consider shaping the product in performing granulation by atomization. In this case, it is more appropriate to put in work this third variant, the granulation being carried out simultaneously with atomization.
Note also that the drying step (in other words, the elimination of molecules of water of crystallization of the mineral salt), can be done simultaneously in the atomizer.
If necessary, it may be advantageous to screen the the composition obtained after drying, to obtain the desired particle size.
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.
12 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.
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.
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.).
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.
Les tensioactifs présentant ces caractéristiques, et choisis, par exemple dans ceux listés auparavant, peuvent être mis en oeuvre en tant que matière active, utilisables notamment dans les domaines de la détergence, de la cosmétique, 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.
Selon une autre possibilité, la formulation peut comprendre au moins une matière active utilisable dans le domaine alimentaire.
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.
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 C$
C22, de préférence en Cep-C2p, contenant de 0 à 30 motifs oxyéthylène. A titre d'exemple de tels composés, conviennent le monolauraté 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 12 All that has just been described with regard to the composition according to the invention, of even that its preparation remains valid and will therefore not be repeated here.
All active ingredients are suitable as long as they are under form anhydrous or include an insufficient amount of water to dissolve the composition according to invention.
The active ingredients can be in liquid form at the setting temperature in form or use, as long as the melting temperature of the active ingredient remains lower than that of the composition; in dispersed / solubilized form in one suitable dispersant / solvent.
These active ingredients can also be formulated. So they can be combined with other compounds such as surfactants, fillers, additives classics in the field in question (anti-foam, etc.).
More particularly, said formulation can comprise at least one material active usable in the areas of detergency, cosmetics, food, plant health or the field of building materials.
Surfactants having these characteristics, and chosen, for example in those listed above can be used as an active ingredient, usable in particular in the fields of detergency, cosmetics, etc.
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.
Alternatively, the formulation may include at least one matter active usable in the food sector.
Among the suitable active ingredients, there may be mentioned flavorings, oils essential, vitamins (such as vitamins A or E), dyes, compounds preventing foaming, such as polyethoxylated oils derived from palm oil, soybean oil, castor oil, rapeseed oil, corn oil, sunflower oil.
We can also cite emulsifiers, stabilizers, thickeners and or gelling agents, chosen from sorbitan esters derived from fatty acids food in C $
C22, preferably in Cep-C2p, containing from 0 to 30 oxyethylene units. As examples of such compounds are suitable sorbitan monolaurate, monooleate sorbitan, sorbitan monopalmitate, sorbitan monostearate, sorbitan tristearate, the polyolethylene sorbitan monolaurant (20 OE), the polyoxyethylene sorbitan monooleate (20 EO), monopalmitate polyoxyethylene sorbitan (20 EO), polyoxyethylene monostearate sorbitan (20 OE), polyoxyethylene sorbitan tristearate (20 OE). Can also be used sodium, potassium, calcium, fatty acids, alone or in combination
13 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 pôlyglycérides d'acides gras alimentaires ; les esters de polypropylène glycol et d'acides gras alimentaires (monoesters ou en mélange avec des diesters) ; le ricinoléate de polyéthylène glycol ;
les esters de polyéthylène glycol et d'acides gras dérivés d'huiles, comme l'huile de soja ; les esters de glycérol et polyéthylène 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.
Selon une autre possibilité, la formulation peut comprendre au moins une matière active utilisable dans le domaine pharmaceutique, les virus, les 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 étre réalisée directement après la préparation de la composition, ou après stockage de la 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.
Si l'opération a eu lieu en présence d'un solvant, on effectue ensuite une étape de séchage du granulé résultant.
II 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.
Dans ce cas, il suffit de mélanger, durant la préparation même de la formulation complexe, en mettant en oeuvre des moyens classiques, la formulation selon l'invention 13 mixtures, obtained from edible fats, or fatty acids distilled foods, mono- and di-glycerides of edible fatty acids, the mono- and di-glycerides of fatty acids esterified by acids carboxylic such as acetic, lactic, citric, tartaric, monoacetyltartaric acids, diacetyltartaric.
Also suitable for sucroesters (esters of fatty acids and sucrose), as well as sucroglycerides which are products obtained by transesterification of synthetic or preferably natural triglycerides speak sucrose. Among the sucroglycerides, there may be mentioned in particular those originating of palm oil, lard, coconut oil, tallow, rapeseed or Castor oil. A procedure for preparing the sucroglycerides is described in French patent application FR 2 463 512. Polyglyceride esters of acids bold food; esters of polypropylene glycol and fatty acids food (monoesters or mixed with diesters); polyethylene ricinoleate glycol;
esters of polyethylene glycol and fatty acids derived from oils, such as oil soy ; esters of glycerol and polyethylene glycol of fatty acids, such as Fatty acids tallow; ethers of polyglycerol and alcohols obtained by reduction of oleic acids and palmitic; fatty acid polyglycerol partial esters of polycondensed castor.
Polysorbates can be advantageously used.
Alternatively, the formulation may include at least one matter active usable in the pharmaceutical field, viruses, enzymes.
The formulation comprising the active ingredient can be obtained by highlighting 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 impregnation of the active material on the composition according to the invention.
The active ingredient is in the form of a liquid, in the form solubilized, in melted form.
If the operation took place in the presence of a solvent, then a stage of drying of the resulting granule.
It should be noted that it would not go beyond the scope of the present invention to using a formulation according to the invention, that is to say comprising the composition and at least an active ingredient, as an additive (adjuvant) to a more complex.
In this case, it suffices to mix, during the very preparation of the formulation complex, using conventional means, the formulation according to the invention
14 (comprenant la composition et au moins une matière active) avec les autres éléments constitutifs de la formulation plus complexe.
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.
Un exemple concret mais non limitatif de l'invention va maintenant être présenté
EXEMPLE
1 ) Préparation de la composition Dans un broyeur Stephan, on introduit 900 g de Na3P04 anhydre (pyrophosphate) 100 g de Geropon~ TA 72 1200 g d'eau (glace).
On broie le mélange pendant la durée nécessaire pour obtenir une poudre.
On effectue ensuite une granulation de la poudre en ajoutant 200 g d'eau.
Les granulés sont séchés dans un lit fluidisé à 110°C pendant une heure puis en étuve, à la même température, pendant 2 heures.
A l'issue du séchage, les granulés ont perdu 6,3 % de leur poids.
2) Absorption d'une matière active 14,4 g de granulés obtenus précédemment (taille inférieure à 400 pm après tamisage) sont mélangés à 9,6 g d'une composition silicone Rhodorsil~ 454 (Rhodia), pendant 10 minutes.
On obtient une poudre sèche, indiquant une bonne imprégnation des granulés.
La teneur en matière active est de 40 % par rapport au 'poids total du granulés. 14 (comprising the composition and at least one active ingredient) with the others elements components of the more complex formulation.
The same could be done by preparing the formulation separately according to the invention (comprising the composition and at least one active material) with others components of the complex formulation to mix them at the time of their use.
A concrete but nonlimiting example of the invention will now be present EXAMPLE
1) Preparation of the composition In a Stephan grinder, we introduce 900 g anhydrous Na3PO4 (pyrophosphate) 100 g Geropon ~ TA 72 1200 g of water (ice).
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.
The granules are dried in a fluidized bed at 110 ° C for one hour then in oven at the same temperature for 2 hours.
After drying, the granules lost 6.3% of their weight.
2) Absorption of an active ingredient 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.
A dry powder is obtained, indicating good impregnation of the granules.
The active ingredient content is 40% relative to the total weight of the granules.
Claims (22)
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 filler is between 0 and 50% by weight of the composition.
at least one surfactant, optionally at least one filler, and water which is located at least in the form of water of crystallization.
.cndot. 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, .cndot. on effectue une granulation du mélange résultant. 15. Preparation process according to the preceding claim, characterized in that the drying of a mixture obtained is carried out in the following way:
.cndot. at least one mineral salt is mixed in anhydrous form or partially hydrated, at least one binder, optionally a surfactant, optionally a load, with the necessary and sufficient quantity of water to hydrate totally said mineral salt, .cndot. the resulting mixture is granulated.
.cndot.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, .cndot.on sèche la solution et/ou la dispersion, .cndot.on effectue une granulation du mélange séché résultant. 17. Process of preparation according to claim 14, characterized in that we performs the following steps:
.cndot.on mixes at least one mineral salt, at least one binder, optionally a surfactant, optionally a filler, with the amount of water necessary to obtain a solution and/or a dispersion, .cndot.on drying the solution and/or the dispersion, .cndot.on performs a granulation of the resulting dried mixture.
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. 20. Formulation according to one of claims 19, characterized in that it is usable as an adjuvant.
21. Process for preparing the formulation according to any one of claims 19 or 20, characterized in that spraying is carried out or a impregnation of the active material, in the form of a liquid, on the composition according to any of claims 1 to 13.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR99/04184 | 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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2365862A1 true CA2365862A1 (en) | 2000-10-12 |
Family
ID=9543987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002365862A Abandoned CA2365862A1 (en) | 1999-04-02 | 2000-04-03 | Mineral-salt based substantially or totally hydrosoluble composition, formulation containing said composition and production thereof |
Country Status (8)
| Country | Link |
|---|---|
| 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) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102015992B (en) | 2008-05-19 | 2012-07-11 | 花王株式会社 | Surfactant-supporting granule cluster |
| FR3037258B1 (en) * | 2015-06-15 | 2020-10-16 | Eurotab | MOISTURE ABSORBING COMPOSITION INCLUDING A SEQUESTRANT AGENT |
| CN110446548B (en) * | 2018-03-06 | 2022-10-11 | 贝赛尔思有限公司 | Method for producing calcium phosphate, and harmful gas and malodor removing composition containing calcium phosphate obtained thereby |
| CN110204354A (en) * | 2019-06-18 | 2019-09-06 | 陈方鑫 | A kind of preparation of quick dephosphorization ceramic particle sorbent material |
| CN113135744B (en) * | 2021-04-02 | 2022-04-01 | 浙江凯色丽科技发展有限公司 | Attapulgite/mica/carbon composite material and preparation method thereof |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3821119A (en) * | 1972-05-03 | 1974-06-28 | Diamond Shamrock Corp | Silicated soda ash |
| GB1466868A (en) * | 1973-04-19 | 1977-03-09 | Unilever Ltd | Granulation of materials |
| PH15690A (en) * | 1979-10-31 | 1983-03-11 | Unilever Nv | Detergent compositions and processes for manufacturing them |
| US4790983A (en) * | 1987-04-24 | 1988-12-13 | Occidental Chemical Corporation | High absorbtivity sodium tripolyphosphate |
| US5294424A (en) * | 1990-06-20 | 1994-03-15 | Monsanto Company | Process for preparing high absorptivity granular sodium phosphates |
| WO1993004154A1 (en) * | 1991-08-20 | 1993-03-04 | Henkel Kommanditgesellschaft Auf Aktien | Method of producing granular carbonate-containing materials |
| WO1993017089A1 (en) * | 1992-02-20 | 1993-09-02 | Henkel Kommanditgesellschaft Auf Aktien | Process for producing low-alkaline dishwasher rinsing agents without active chlorine, silicates and phosphates, in the form of heavy granulates |
| US5733862A (en) * | 1993-08-27 | 1998-03-31 | The Procter & Gamble Company | Process for making a high density detergent composition from a sufactant paste containing a non-aqueous binder |
| AU4782897A (en) * | 1997-11-07 | 1999-05-31 | Fmc Foret, S.A. | Homogenous granules comprised of sodium tripolyphosphate, sodium sulphate and sodium carbonate, process for its preparation and applications to detergents and washing agents |
-
1999
- 1999-04-02 FR FR9904184A patent/FR2791581B1/en not_active Expired - Fee Related
-
2000
- 2000-04-03 CA CA002365862A patent/CA2365862A1/en not_active Abandoned
- 2000-04-03 WO PCT/FR2000/000834 patent/WO2000059628A1/en active Search and Examination
- 2000-04-03 AU AU38236/00A patent/AU3823600A/en not_active Abandoned
- 2000-04-03 BR BR0009538-9A patent/BR0009538A/en not_active IP Right Cessation
- 2000-04-03 EP EP00917117A patent/EP1183100A1/en not_active Withdrawn
- 2000-04-03 JP JP2000609182A patent/JP2002541267A/en active Pending
-
2001
- 2001-09-27 ZA ZA200107945A patent/ZA200107945B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| EP1183100A1 (en) | 2002-03-06 |
| FR2791581B1 (en) | 2001-05-18 |
| FR2791581A1 (en) | 2000-10-06 |
| WO2000059628A1 (en) | 2000-10-12 |
| ZA200107945B (en) | 2002-05-08 |
| JP2002541267A (en) | 2002-12-03 |
| BR0009538A (en) | 2003-03-05 |
| AU3823600A (en) | 2000-10-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| FZDE | Discontinued |