FR2672294A1 - Process for the preparation of a composition based on synthetic thickeners - Google Patents
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- FR2672294A1 FR2672294A1 FR9101150A FR9101150A FR2672294A1 FR 2672294 A1 FR2672294 A1 FR 2672294A1 FR 9101150 A FR9101150 A FR 9101150A FR 9101150 A FR9101150 A FR 9101150A FR 2672294 A1 FR2672294 A1 FR 2672294A1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/005—Processes for mixing polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
- C10M119/04—Lubricating compositions characterised by the thickener being a macromolecular compound containing oxygen
- C10M119/06—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M119/12—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
- C10M119/04—Lubricating compositions characterised by the thickener being a macromolecular compound containing oxygen
- C10M119/14—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
- C10M119/24—Lubricating compositions characterised by the thickener being a macromolecular compound containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/0813—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/084—Acrylate; Methacrylate
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/086—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type polycarboxylic, e.g. maleic acid
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/086—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type polycarboxylic, e.g. maleic acid
- C10M2209/0866—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type polycarboxylic, e.g. maleic acid used as thickening agents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/024—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
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Abstract
Description
La présente invention a pour objet un procédé de préparation d'une composition à base d'épaississants synthétiques se présentant sous une forme liquide et translucide et possédant une bonne stabilité au stockage. The present invention relates to a process for the preparation of a composition based on synthetic thickeners in a liquid and translucent form and having good storage stability.
L'emploi de composés permettant d'épaissir des solutions aqueuses est fréquent dans de nombreux secteurs de l'industrie, notamment dans l'industrie textile, afin de réaliser l'épaississement des couleurs d'impression. The use of compounds making it possible to thicken aqueous solutions is frequent in many industrial sectors, in particular in the textile industry, in order to thicken the printing colors.
L'emploi de composés épaississants naturels tels que des alginates ou dérivés cellulosiques, a été longtemps pratiqué. Toutefois, l'usage d'épaississants synthétiques est de plus en plus préféré en raison de leurs caractéristiques particulières, notamment de leur pouvoir épaississant plus élevé que celui des produits naturels. The use of natural thickening compounds such as alginates or cellulose derivatives has long been practiced. However, the use of synthetic thickeners is increasingly preferred because of their particular characteristics, in particular their thickening power which is higher than that of natural products.
Un certain nombre de composés, polymères ou copolymères, sont actuellement en faveur sur le marché des épaississants. On peut citer, notamment, des polyacrylates, des polymères de l'acide acrylique, ainsi que des copolymères, tels que les copolymères d'éthylène et d'anhydride maléique. A certain number of compounds, polymers or copolymers, are currently in favor on the market of thickeners. There may be mentioned, in particular, polyacrylates, polymers of acrylic acid, as well as copolymers, such as copolymers of ethylene and maleic anhydride.
La mise en oeuvre et/ou la manipulation de produits se présentant sous la forme de poudre fine n'étant jamais facile, la commercialisation des épaississants synthétiques est désormais plus fréquemment réalisée sous la forme de pâtes de viscosité plus ou moins importante. Since the implementation and / or handling of products in the form of fine powder is never easy, the marketing of synthetic thickeners is now more frequently carried out in the form of pastes of greater or lesser viscosity.
La préparation de ces pâtes est effectuée actuellement selon deux procédés
Un premier procédé consiste à disperser une poudre, par exemple d'acide polyacrylique, dans un liquide fréquemment constitué d'un mélange d'eau et d'un solvant organique, additionné d'un émulsionnant approprié. La réalisation d'une telle dispersion soulève cependant de nombreuses difficultés et ne permet d'obtenir que des dispersions relativement grossières conduisant à des produits se présentant sous la forme de pâtes plus ou moins visqueuses dont la stabilité est imparfaite. On observe en particulier, au cours du temps, une séparation des différentes phases constituant le produit, ce qui nécessite, avant emploi, de les soumettre à une vive agitation.The preparation of these pastas is currently carried out according to two methods
A first method consists in dispersing a powder, for example polyacrylic acid, in a liquid frequently consisting of a mixture of water and an organic solvent, added with a suitable emulsifier. The production of such a dispersion, however, raises many difficulties and makes it possible to obtain only relatively coarse dispersions leading to products in the form of more or less viscous pastes whose stability is imperfect. We observe in particular, over time, a separation of the different phases constituting the product, which requires, before use, to subject them to vigorous stirring.
Un deuxième procédé consiste à réaliser une émulsion du polymère ou copolymère épaississant par le procédé de polymérisation en phase inverse décrit dans différentes publications, par exemple par J.W. Vanderhoff et al.,
Advances In Chemistry Series, N0 34, (1961), pages 32 et suivantes.Ce procédé permet d'obtenir une amélioration de la stabilité et de la fluidité de l'épaississant sans cependant permettre d'obtenir une stabilité parfaite de l'émulsion au cours du temps
Il a été observé par la Demanderesse que l'introduction d'un polymère ou d'un copolymère en poudre dans une émulsion d'un polymère ou copolymère obtenu par polymérisation en phase inverse, permet de disperser rapidement la poudre sans rencontrer les difficultés habituellement rencontrées dans ce type d'opérations et permet d'obtenir facilement des dispersions très fines de la poudre introduite, conduisant en particulier à l'obtention de produits épaississants se présentant sous une forme liquide et parfaitement translucide.A second process consists in producing an emulsion of the thickening polymer or copolymer by the reverse phase polymerization process described in various publications, for example by JW Vanderhoff et al.,
Advances In Chemistry Series, N0 34, (1961), pages 32 et seq. This process makes it possible to obtain an improvement in the stability and the fluidity of the thickener without however making it possible to obtain perfect stability of the emulsion course of time
It has been observed by the Applicant that the introduction of a polymer or a powdered copolymer into an emulsion of a polymer or copolymer obtained by reverse phase polymerization makes it possible to rapidly disperse the powder without encountering the difficulties usually encountered. in this type of operation and makes it possible to easily obtain very fine dispersions of the powder introduced, leading in particular to obtaining thickening products which are in a liquid and perfectly translucent form.
Il est apparu également que l'introduction d'une poudre dans une émulsion obtenue par polymérisation en phase inverse, permet d'introduire des quantités plus importantes de poudre que par le procédé actuellement utilisé faisant usage d'un mélange d'eau et de solvant organique, sans risque de prise en masse de l'ensemble et en permettant d'obtenir des produits liquides et translucides, d'une bonne stabilité. It also appeared that the introduction of a powder into an emulsion obtained by reverse phase polymerization, makes it possible to introduce larger quantities of powder than by the process currently used using a mixture of water and solvent organic, without risk of solidification of the whole and making it possible to obtain liquid and translucent products, of good stability.
Comparés aux émulsions ou dispersions des épaississants réalisés selon les procédés antérieurs, les produits résultant du procédé de l'invention se distinguent par les avantages suivants
- un aspect liquide et translucide facilitant leur mise en oeuvre en permettant par exemple l'emploi de pompes ou d'appareils de distribution automatique du produit
- une plus grande stabilité des produits au stockage
- une concentration en produit épaississant, polymère ou copolymère, ou un pouvoir épaississant comparativement plus élevé que celui des produits actuels, caractéristiques importantes se traduisant par des avantages économiques et/ou écologiques intéressants résultant par exemple d'une diminution possible du nombre des emballages, de la réduction des frais de stockage, de transport, de lavage ou recyclage des emballages, voire encore de moindres pertes résiduelles dans les emballages en raison de la fluidité des produits ; et
- la possibilité de formuler des épaississants constitués d'un mélange de différents polymères et/ou copolymères, cette possibilité permettant d'améliorer un certain nombre de caractéristiques, telles que
. le pouvoir épaississant,
l'influence du produit sur un support, par exemple moindre modification de la souplesse d'une fibre,
une moindre sensibilité aux électrolytes, et
. une meilleure résistance aux effets mécaniques.Compared with the emulsions or dispersions of thickeners produced according to the previous processes, the products resulting from the process of the invention are distinguished by the following advantages
- a liquid and translucent appearance facilitating their implementation by allowing for example the use of pumps or automatic product dispensing devices
- greater stability of products during storage
a concentration of thickening product, polymer or copolymer, or a comparatively higher thickening power than that of current products, important characteristics resulting in advantageous economic and / or ecological advantages resulting for example from a possible reduction in the number of packages, reducing the costs of storing, transporting, washing or recycling the packaging, or even lower residual losses in the packaging due to the fluidity of the products; and
the possibility of formulating thickeners consisting of a mixture of different polymers and / or copolymers, this possibility making it possible to improve a certain number of characteristics, such as
. thickening power,
the influence of the product on a support, for example less modification of the flexibility of a fiber,
less sensitivity to electrolytes, and
. better resistance to mechanical effects.
La présente invention concerne donc un procédé de préparation d'une composition épaississante à base de polymères synthétiques doués de propriétés épaississantes caractérisé en ce qu'il consiste à disperser une poudre d'un premier polymère doué de propriétés épaississantes dans une émulsion, préparée par polymérisation en phase inverse, d'un deuxième polymère doué de propriétés épaississantes, puis à régler le pH de la dispersion résultante dans la gamme de 6 à 8. The present invention therefore relates to a process for the preparation of a thickening composition based on synthetic polymers endowed with thickening properties, characterized in that it consists in dispersing a powder of a first polymer endowed with thickening properties in an emulsion, prepared by polymerization. in the reverse phase, a second polymer endowed with thickening properties, then adjusting the pH of the resulting dispersion in the range of 6 to 8.
La présente invention concerne aussi une composition épaississante, liquide, translucide et stable, à base de polymères synthétiques, caractérisée en ce qu'elle est constituée de particules d'un premier polymère doué de propriétés épaississantes dispersées dans une émulsion d'un deuxième polymère doué de propriétés épaississantes, ladite émulsion ayant été préparée par polymérisation en phase inverse, et ledit premier polymère étant sous la forme de son sel d'ammonium, de sodium ou de potassium. The present invention also relates to a thickening, liquid, translucent and stable composition, based on synthetic polymers, characterized in that it consists of particles of a first polymer endowed with thickening properties dispersed in an emulsion of a second end polymer thickening properties, said emulsion having been prepared by reverse phase polymerization, and said first polymer being in the form of its ammonium, sodium or potassium salt.
Par "polymère" on entend aussi bien un homopolymère qu'un copolymère
Le premier et le deuxième polymères peuvent être identiques ou différents.By "polymer" is meant both a homopolymer and a copolymer
The first and second polymers can be the same or different.
Le premier polymère peut être constitué d'un des polymères connus couramment utilisés pour épaissir des solutions aqueuses. A titre indicatif et non limitatif, on peut citer, par exemple, de façon non limitative, un polymère d'acide acrylique ou un copolymère éthylèneanhydride maléique. The first polymer can consist of one of the known polymers commonly used to thicken aqueous solutions. By way of indication and without limitation, mention may be made, for example, without limitation, of an acrylic acid polymer or an ethylene maleic anhydride copolymer.
Par l'expression "poudre d'un premier polymère", on entend aussi bien une poudre sèche qu'une poudre humide, c'est-à-dire un mélange de particules dudit premier polymère et d'un milieu organique liquide non solvant dudit premier polymère, y compris une dispersion desdites particules dans ledit milieu organique liquide non solvant. Lorsqu ' on utilise une poudre humide, il peut y avoir lieu de procéder à une opération de distillation après dispersion de la poudre, pour éliminer ledit milieu organique non solvant, notamment lorsque ce dernier présente des risques d'inflammabilité ou de toxicité. By the expression "powder of a first polymer" is meant both a dry powder and a wet powder, that is to say a mixture of particles of said first polymer and of a non-solvent liquid organic medium of said first polymer, including a dispersion of said particles in said non-solvent liquid organic medium. When a wet powder is used, it may be necessary to carry out a distillation operation after dispersion of the powder, in order to eliminate said non-solvent organic medium, in particular when the latter presents risks of flammability or toxicity.
L'émulsion préparée par polymérisation en phase inverse, comprend un deuxième polymère doué de propriétés épaississantes et dérivant d'au moins un monomère éthyléniquement insaturé soluble dans l'eau, tel que par exemple un polyacrylamide, un copolymère acrylamide/acrylonitrile ou acrylamide/acrylate, un polyacrylate, et un polymère ou copolymère de 1 ' acide acrylique. The emulsion prepared by reverse phase polymerization comprises a second polymer endowed with thickening properties and derived from at least one ethylenically unsaturated water-soluble monomer, such as for example a polyacrylamide, an acrylamide / acrylonitrile or acrylamide / acrylate copolymer. , a polyacrylate, and a polymer or copolymer of acrylic acid.
La dispersion de la poudre du premier polymère dans 1 'émulsion du deuxième polymère, obtenue par polymérisation en phase inverse, peut être effectuée en introduisant progressivement la poudre du premier polymère dans l'émulsion maintenue sous vive agitation et à la température ambiante (20-25 C) afin de disperser la poudre et obtenir rapidement un mélange homogène. The powder of the first polymer is dispersed in the emulsion of the second polymer, obtained by reverse phase polymerization, can be carried out by gradually introducing the powder of the first polymer into the emulsion maintained under vigorous stirring and at room temperature (20- C) in order to disperse the powder and quickly obtain a homogeneous mixture.
Une fois cette dispersion réalisée, on règle le pH de la dispersion à une valeur de 6 à 8 au moyen d'une base, telle que l'hydroxyde d'ammonium, de sodium ou de potassium. Cette addition de base a pour effet de neutraliser l'acidité du ou des polymère(s) acide(s) présents avec formation d'un sel, tel que le sel d'ammonium, de sodium ou de potassium, du premier polymère et, le cas échéant, du deuxième polymère. On préfère tout particulièrement utiliser l'hydroxyde d'ammonium (ammoniaque) comme base, car c'est cette dernière qui permet d'obtenir une composition ayant les meilleures propriétés épaississantes. Once this dispersion has been carried out, the pH of the dispersion is adjusted to a value of 6 to 8 by means of a base, such as ammonium, sodium or potassium hydroxide. This addition of base has the effect of neutralizing the acidity of the acidic polymer (s) present with the formation of a salt, such as the ammonium, sodium or potassium salt, of the first polymer and, where appropriate, the second polymer. It is particularly preferred to use ammonium hydroxide (ammonia) as the base, because it is the latter which makes it possible to obtain a composition having the best thickening properties.
La quantité du premier polymère pouvant être introduite dans l'émulsion du deuxième polymère servant de dispersant variera en fonction des caractéristiques désirées pour la composition finale. A titre indicatif, cette quantité sera habituellement comprise entre 1 et 150% en poids, de préférence de 30 à 80% en poids, de premier polymère par rapport à la quantité d'émulsion du deuxième polymère mise en oeuvre. The amount of the first polymer that can be introduced into the emulsion of the second polymer serving as a dispersant will vary depending on the characteristics desired for the final composition. As an indication, this amount will usually be between 1 and 150% by weight, preferably 30 to 80% by weight, of the first polymer relative to the amount of emulsion of the second polymer used.
En plus des avantages précédemment cités, la présente invention offre, en outre, l'avantage, par le choix des polymères utilisés, de permettre d'ajuster le pouvoir épaississant de la composition épaississante finalement obtenue. In addition to the advantages mentioned above, the present invention also offers the advantage, by the choice of polymers used, of making it possible to adjust the thickening power of the thickening composition finally obtained.
Les exemples non limitatifs ci-après sont donnés afin d'illustrer de façon plus concrète la présente invention
EXEMPLE 1
On prépare une émulsion de copolymère d'acrylamide (15% en poids) et d'acide acrylique (85t en poids) par polymérisation en phase inverse. The following nonlimiting examples are given in order to illustrate the present invention more concretely.
EXAMPLE 1
An emulsion of acrylamide copolymer (15% by weight) and acrylic acid (85t by weight) is prepared by reverse phase polymerization.
A la fin de l'opération on obtient une émulsion contenant 50% en poids dudit copolymère. At the end of the operation, an emulsion containing 50% by weight of said copolymer is obtained.
Dans 500 g de l'émulsion obtenue, maintenue sous agitation, on introduit 200 g d'une poudre d'acide polyacrylique de haut poids moléculaire. On obtient très rapidement une dispersion de la poudre dans l'émulsion. 200 g of a polyacrylic acid powder of high molecular weight are introduced into 500 g of the emulsion obtained, kept under stirring. A dispersion of the powder in the emulsion is very quickly obtained.
On introduit ensuite rapidement 300 g d'une solution d'ammoniaque à 30% afin de former le sel d'ammonium de l'acide polyacrylique. 300 g of a 30% ammonia solution are then rapidly introduced in order to form the ammonium salt of polyacrylic acid.
On obtient un liquide de couleur jaune, translucide et d'excellente stabilité, contenant au total 45% de matière sèche ou 40% d'acide polyacrylique par rapport à la quantité d'émulsion introduite, et présentant un pH compris dans la gamme de 6 à 8. A yellow, translucent liquid of excellent stability is obtained, containing a total of 45% dry matter or 40% polyacrylic acid relative to the amount of emulsion introduced, and having a pH in the range of 6 at 8.
Comparativement, l'introduction d'une même quantité d'acide polyacrylique dans un mélange eau/solvant organique additionné d'émulsionnants, ou dans une huile minérale additionnée d'émulsionnants, s'avère longue et difficile. On observe, en outre, ensuite, après l'addition d'ammoniaque, un risque très important de prise en masse. Comparatively, the introduction of the same amount of polyacrylic acid in a water / organic solvent mixture added with emulsifiers, or in a mineral oil added with emulsifiers, proves to be long and difficult. In addition, there is then observed, after the addition of ammonia, a very significant risk of solidification.
On aboutit finalement, dans le meilleur des cas, à un produit pâteux, grossièrement dispersé et rapidement instable.At the end of the day, in the best of cases, a pasty product, roughly dispersed and rapidly unstable.
On prépare trois compositions épaississantes diluées, en dispersant dans l'eau, 20 g/l de chacun des trois produits ci-dessous. Les viscosités des compositions diluées sont les suivantes
- émulsion de copolymère d'acrylamide et d'acrylate de sodium contenant 50% en poids du copolymère = 20 000 mPa,
- dispersion d'acide polyacrylique dans un mélange eau/solvant organique contenant 20% en poids de polymère = 18 000 mPa,
- dispersion selon l'invention contenant 45% en poids de polymères totaux = 32 000 mPa.Three diluted thickening compositions are prepared, by dispersing in water, 20 g / l of each of the three products below. The viscosities of the diluted compositions are as follows
- emulsion of acrylamide and sodium acrylate copolymer containing 50% by weight of the copolymer = 20,000 mPa,
- dispersion of polyacrylic acid in a water / organic solvent mixture containing 20% by weight of polymer = 18,000 mPa,
- dispersion according to the invention containing 45% by weight of total polymers = 32,000 mPa.
On observe que l'épaississant selon l'invention permet d'obtenir une viscosité nettement plus élevée bien que sa teneur en polymères soit inférieure à celle de l'émulsion de copolymère acrylamide-acrylate de sodium. It is observed that the thickener according to the invention makes it possible to obtain a significantly higher viscosity although its polymer content is lower than that of the emulsion of acrylamide-sodium acrylate copolymer.
EXEMPLE 2
On introduit dans 200 g de l'émulsion de l'exemple 1 maintenue sous agitation, 200 g d'une huile minérale dont le point d'ébullition est supérieur à 2000C puis 300 g de la poudre d'acide polyacrylique de l'exemple 1. On obtient très rapidement une très fine dispersion de la poudre.EXAMPLE 2
200 g of the emulsion of example 1 kept stirred are introduced into 200 g of a mineral oil whose boiling point is above 2000 ° C. and then 300 g of the polyacrylic acid powder of example 1 A very fine dispersion of the powder is very quickly obtained.
On introduit ensuite 200 g d'une solution d'ammoniaque à 30%. On obtient un liquide de couleur jaune, translucide, d'un pH de 6 à 8, et parfaitement stable au stockage dont la teneur en polymères est de 40% en poids et dont la quantité d'acide polyacrylique est de 150% par rapport au poids de l'émulsion. 200 g of a 30% ammonia solution are then introduced. A yellow, translucent liquid with a pH of 6 to 8 is obtained, which is perfectly stable on storage, the polymer content of which is 40% by weight and the amount of polyacrylic acid is 150% relative to the weight of the emulsion.
Comme dans l'exemple 1, la détermination des viscosités réalisée sur les différents produits permet d'observer un pouvoir épaississant très nettement plus élevé avec la composition selon l'invention. As in Example 1, the determination of the viscosities carried out on the various products makes it possible to observe a very markedly higher thickening power with the composition according to the invention.
Les résultats enregistrés sont en effet
- émulsion de copolymère acrylamide-acrylate de sodium contenant 50% en poids du copolymère : 20 000 mPa,
- émulsion selon l'invention contenant 40% en poids de polymères totaux : 36 000 mPa.The results recorded are indeed
- emulsion of acrylamide-sodium acrylate copolymer containing 50% by weight of the copolymer: 20,000 mPa,
- emulsion according to the invention containing 40% by weight of total polymers: 36,000 mPa.
EXEMPLE 3
Dans 500 g de l'émulsion utilisée dans l'exemple 1 on introduit, sous agitation, 200 g d'une poudre de copolymère éthylène/anhydride maléique.EXAMPLE 3
200 g of an ethylene / maleic anhydride copolymer powder are introduced into 500 g of the emulsion used in Example 1, with stirring.
On obtient très rapidement une fine dispersion de la poudre. On introduit ensuite, afin de produire le sel d'ammonium, 300 g d'ammoniaque à 30%. A fine dispersion of the powder is very quickly obtained. Then, in order to produce the ammonium salt, 300 g of 30% ammonia are introduced.
On obtient un liquide de couleur jaune, translucide, d'un pH de 6 à 8, de bonne stabilité au stockage et possédant un excellent pouvoir épaississant. A yellow, translucent liquid with a pH of 6 to 8 is obtained, with good storage stability and having an excellent thickening power.
EXEMPLE 4
On prépare par polymérisation une dispersion de 20% en poids d'acide polyacrylique de haut poids moléculaire dans du benzène. EXAMPLE 4
A dispersion of 20% by weight of high molecular weight polyacrylic acid in benzene is prepared by polymerization.
On introduit dans 100 g de cette dispersion maintenue sous agitation, 500 g de l'émulsion de l'exemple 1 puis 300 g d'une solution d'ammoniaque à 30%. 500 g of the emulsion of Example 1 and then 300 g of a 30% ammonia solution are introduced into 100 g of this dispersion, with stirring.
On distille ensuite, en opérant sous vide, la quantité totale de benzène présent dans le mélange. Then distilled, operating under vacuum, the total amount of benzene present in the mixture.
Après distillation, on obtient un liquide doué de bonnes propriétés épaississantes, relativement visqueux, d'un pH de 6 à 8, de couleur jaune et translucide, possédant une excellente stabilité au stockage. After distillation, a liquid with good thickening properties, relatively viscous, with a pH of 6 to 8, of yellow and translucent color, having excellent storage stability, is obtained.
Claims (11)
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FR9101150A FR2672294B1 (en) | 1991-02-01 | 1991-02-01 | PROCESS FOR THE PREPARATION OF A COMPOSITION BASED ON SYNTHETIC THICKENERS. |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS502170B1 (en) * | 1970-10-30 | 1975-01-24 | ||
USRE28576E (en) * | 1970-12-15 | 1975-10-21 | Process for rapid dissolving water-soluble vinyl addition polymers using water-in-oil emulsions | |
EP0169674B1 (en) * | 1984-06-28 | 1990-05-09 | Ciba Specialty Chemicals Water Treatments Limited | Polymer powders |
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1991
- 1991-02-01 FR FR9101150A patent/FR2672294B1/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS502170B1 (en) * | 1970-10-30 | 1975-01-24 | ||
USRE28576E (en) * | 1970-12-15 | 1975-10-21 | Process for rapid dissolving water-soluble vinyl addition polymers using water-in-oil emulsions | |
USRE28576F1 (en) * | 1970-12-15 | 1983-12-06 | ||
EP0169674B1 (en) * | 1984-06-28 | 1990-05-09 | Ciba Specialty Chemicals Water Treatments Limited | Polymer powders |
Non-Patent Citations (1)
Title |
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BASE DE DONNEES WPI, accession no. 75-13611W, Derwent Publications Ltd, Londres, GB; & JP-B-50 002 170 (TOA GOSEI CHEM. IND. CO.) 24-01-1975 * |
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