EP4565646A2 - Compositions de suspension fluide stable sans sel aqueux et leur procédé de préparation - Google Patents

Compositions de suspension fluide stable sans sel aqueux et leur procédé de préparation

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Publication number
EP4565646A2
EP4565646A2 EP23850850.1A EP23850850A EP4565646A2 EP 4565646 A2 EP4565646 A2 EP 4565646A2 EP 23850850 A EP23850850 A EP 23850850A EP 4565646 A2 EP4565646 A2 EP 4565646A2
Authority
EP
European Patent Office
Prior art keywords
composition according
combinations
group
composition
cellulose ether
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.)
Pending
Application number
EP23850850.1A
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German (de)
English (en)
Inventor
Joachim Krause
Michael Dittel
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Hercules LLC
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Hercules LLC
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Publication date
Application filed by Hercules LLC filed Critical Hercules LLC
Publication of EP4565646A2 publication Critical patent/EP4565646A2/fr
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/08—Cellulose derivatives
    • C09D101/26—Cellulose ethers
    • C09D101/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J101/00—Adhesives based on cellulose, modified cellulose, or cellulose derivatives
    • C09J101/08—Cellulose derivatives
    • C09J101/26—Cellulose ethers
    • C09J101/28—Alkyl ethers

Definitions

  • This invention relates to the stable fluid suspension compositions and particularly, relates to an aqueous based, salt-free, stable fluid suspension composition comprising at least one cellulose ether and at least one salt-free insolubilizing agent.
  • Cellulose ether polymers are the most commonly used rheology modifiers in aqueous based formulations. It is generally supplied in the powder form, which are then subsequently dissolved into various water-based systems to achieve desired rheology profiles. Processing difficulties were encountered while incorporating and dispersing said cellulosic ether powders into water-containing liquid formulations and often tend to form lumps when added to water-based systems. When the water soluble polymer powder is added in bulk, particles at the interface between powder phase and fluid phase of such water-based systems begin to rapidly hydrate and swell and causes particle jamming at the interface and slows down fluid penetration into the interior of the powder phase. This process ultimately results in the formation of persistent, slowly dissolving gel agglomerates of various sizes and adversely affect the rate of dissolution.
  • U.S. Pat. No. 4,469,627 filed by Colgate Palmolive Co discloses a process for dispersing hydroxypropyl methyl cellulose in a nonaqueous liquified organic medium in which it does not swell or dissolve, and subsequently adding said dispersion to an aqueous-containing liquid formulation wherein it is readily solubilized.
  • U.S. Pat. No. 4,883,536 filed by Aquaion discloses fluid polymer suspensions of cellulosic polymers using ammonium salts having multivalent anions.
  • U.S. Patent 4,283,229 filed by Hoechst AG discloses, a process for the preparation of a stable aqueous cellulose ether suspension which contains an electrolyte, and to the use of such a suspension.
  • U.S. Patent 4,883,537 filed by Aquaion discloses stable aqueous suspensions of water- soluble carboxymethylcellulose, a process for preparing the same, and use of the same in a variety of applications.
  • U.S. Patent 6,025,311 filed by Aquaion discloses the use of aqueous fluid suspensions of polysaccharides in cosmetic, personal care and household applications.
  • the concentration of inorganic salts must be adjusted such that the flocculation (or cloud) point, i.e., the temperature at which a polymer precipitates or gels from solution to render a cloudy dispersion, is below room temperature.
  • the concentration of inorganic salts in the fluid polymer suspension must be sufficiently high to render the hydrophilic cellulose ether polymer insoluble in the salt water in a temperature at which the fluid polymer suspension is to be stored and used.
  • inorganic salts in the fluidized polymer suspension is highly undesirable for some specialty applications which may include, but not limited to, washcoats, drilling fluids, specialty coatings, household products and agricultural products. It may interfere and interact with other additives such as metal particles within the formulation or, may lead to some unwanted chemical reactions with substrates, like poisoning catalytic activities or other materials/fluids it may come in contact with, during the end-user application. These inorganic salts also leave some residues on the substrates/surfaces it is coated to, and not completely removable during calcination, which is highly undesirable for specialty coating applications such as washcoats.
  • the primary aspect of the present application is to provide an aqueous salt-free fluid suspension composition
  • an aqueous salt-free fluid suspension composition comprising: (i) about 0.01 wt.% to about 30 wt.% of at least one cellulose ether, (ii) about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof, (iii) about 0.01 wt.% to about 5 wt.% of at least one stabilizing agent, (iv) about 0.01 wt.% to about 5 wt.% of at least one preservative, and (v) about 0.01 wt.% to about 70 wt.% of water.
  • the cellulose ether is selected from the group consisting of methylhydroxypropylcellulose (MHPC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), carboxymethylhydroxyethylcellulose (CMHEC), hydroxyethylcellulose (HEC), hydrophobically modified hydroxyethylcellulose (HMHEC), ethylhydroxyethylcellulose (EHEC), hydrophobically modified ethylhydroxyethylcellulose (HMEHEC), methylhydroxyethylcellulose (MHEC), and combinations thereof.
  • MHPC methylhydroxypropylcellulose
  • HPC hydroxypropylcellulose
  • HPC methylcellulose
  • CMC carboxymethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • HEC hydroxyethylcellulose
  • HHEC hydrophobically modified hydroxyethylcellulose
  • EHEC
  • the methylhydroxypropylcellulose (MHPC) has a degree of polymerization (D.P.) value ranging from about 600 to about 2200 and, hydroxypropylcellulose (HPC) has a degree of polymerization (D.P.) value ranging from about 600 to about 2200.
  • the methylhydroxypropylcellulose has a methoxy content ranging from about 25% to about 35% and a propoxy content ranging from about 5% to about 15%.
  • the hydroxypropylcellulose has a molar substitution (M.S.) value ranging from about 3 to about 5.
  • the monosaccharide is selected from the group consisting of glucose, dextrose, fructose, galactose, xylose, ribose, and combinations thereof;
  • the disaccharide is selected from the group consisting of sucrose, lactose, maltose, lactulose, trehalose, and combinations thereof;
  • the polysaccharide is selected from the group consisting of maltodextrin, starch, amylose, amylopectin, dextran, and combinations thereof.
  • Another aspect of the present application discloses a process for preparing an aqueous salt-free fluid suspension composition, wherein the process comprising the steps of:
  • step (b) adding about 0.01 wt.% to about 5 wt.% of least one stabilizing agent into the reaction container of step (a); (c) adding about 0.01 wt.% to about 5 wt.% of at least one preservative into the resultant of step (b);
  • step (d) adding about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent into the resultant of step (c) and continuing the agitation to achieve complete dissolution;
  • step (e) adding about 0.01 wt.% to about 30 wt.% of at least one cellulose ether into the resultant of step (d) and continuing the agitation till obtaining a homogenized fluid suspension composition.
  • a thickening composition comprising an aqueous salt-free fluid suspension composition comprising: (i) about 0.01 wt.% to about 30 wt.% of at least one cellulose ether, (ii) about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof, (iii) about 0.01 wt.% to about 5 wt.% of at least one stabilizing agent, (iv) about 0.01 wt.% to about 5 wt.% of at least one preservative, and (v) about 0.01 wt.% to about 70 wt.% of water.
  • FIG. 1 illustrates the dissolution behavior of fluidized polymer suspension based on MHPC against typical dry cellulose ether powder (Natrosol 250MRHEC) suspended in an aqueous solution at pH 3 and at ambient temperature.
  • FIG. 2 illustrates the dissolution behavior of fluidized polymer suspension based on MHPC against typical dry cellulose ether powder (Natrosol 250MRHEC) suspended in an aqueous solution at pH 7 and at ambient temperature.
  • FIG. 3 illustrates the dissolution behavior of fluidized polymer suspension based on MHPC against typical dry cellulose ether powder (Natrosol 250MRHEC) suspended in an aqueous solution at pH 11 and at ambient temperature.
  • FIG. 4 illustrates the dissolution behavior of fluidized polymer suspension based on MHPC against typical dry cellulose ether powder (Culminal MHEC 6000PR) suspended in an aqueous solution at pH 3 and at ambient temperature.
  • FIG. 5 illustrates the dissolution behavior of fluidized polymer suspension based on MHPC against typical dry cellulose ether powder (Culminal MHEC 6000PR) suspended in an aqueous solution at pH 7 and at ambient temperature.
  • At least one will be understood to include one as well as any quantity more than one, including but not limited to, 1, 2, 3, 4, 5, 10, 15, 20, 30, 40, 50, 100, etc.
  • the term “at least one” may extend up to 100 or 1000 or more depending on the term to which it is attached. In addition, the quantities of 100/1000 are not to be considered limiting as lower or higher limits may also produce satisfactory results.
  • the words “comprising” (and any form of comprising, such as “comprise” and “comprises”), “having” (and any form of having, such as “have” and “has”), “including” (and any form of including, such as “includes” and “include”) or “containing” (and any form of containing, such as “contains” and “contain”) are inclusive or open-ended and do not exclude additional, unrecited elements or method steps.
  • each independently selected from the group consisting of means when a group appears more than once in a structure, that group may be selected independently each time it appears.
  • Inverted sugar describes a liquified form of table sugar in which the chemical bonds between glucose and fructose molecules have been broken, produced commercially by acidic or enzymatic hydrolysis. It is resistant to crystallization and promotes retention of moisture.
  • the “Inverted sugar” consists of “active dry substance content” hereinafter referred as “active content” and “conversion rate of the sugar” hereinafter referred as “conversion rate” hereinafter.
  • active content active dry substance content
  • conversion rate conversion rate
  • the inverted sugar syrup 72.7/66 consists of 72.7% dry substance and 66% inverted sugar, therefore 34% saccharose.
  • the present disclosure is directed to an aqueous salt-free fluid suspension composition
  • an aqueous salt-free fluid suspension composition comprising: (i) about 0.01 wt.% to about 30 wt.% of at least one cellulose ether, (ii) about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof, (iii) about 0 01 wt.% to about 5 wt.% of at least one stabilizing agent, (iv) about 0.01 wt.% to about 5 wt.% of at least one preservative, and (v) about 0.01 wt.% to about 70 wt.% of water.
  • the cellulose ether of the present invention is selected from the group consisting of methylhydroxypropylcellulose (MHPC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), carboxymethylhydroxyethylcellulose (CMHEC), hydroxyethylcellulose (HEC), hydrophobically modified hydroxy ethylcellulose (HMHEC), ethylhydroxy ethylcellulose (EHEC), hydrophobically modified ethylhydroxyethylcellulose (HMEHEC), methylhydroxyethylcellulose ( H EC ), and combinations thereof.
  • MHPC methylhydroxypropylcellulose
  • HPC hydroxypropylcellulose
  • MC carboxymethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • HEC hydroxyethylcellulose
  • HMEHEC hydrophobically modified hydroxyethylcellulose
  • the methylhydroxypropylcellulose has a degree of polymerization (D.P.) value ranging from about 600 to about 800; or from about 800 to about 1000; or from about 1000 to about 1200; or from about 1200 to about 1400; or from about 1400 to about 1600; or from about 1600 to about 1800; or from about 1800 to about 2000; or from about 2000 to about 2200.
  • D.P. degree of polymerization
  • the molar substitution (M.S.) of methylhydroxypropylcellulose (MHPC) comprises: a methoxy content ranging from about 25% to about 27%; or from about 27% to about 29%; or from about 29% to about 31%; or from about 31% to about 33%; or from about 33% to about 35%; and a propoxy content ranging from about 5% to about 7%; or from about 7% to about 9%; or from about 9% to about 11%; or from about 11% to about 13%; or from about 13% to about 15%.
  • the Hydroxypropylcellulose (HPC) of the present invention having a molar substitution (M.S ) value ranging from about 3 to about 3.5; or from about 3.5 to about 4; or from about 4 to about 4.5; or from about 4.5 to about 5.
  • the hydroxypropylcellulose has a degree of polymerization (D.P.) value ranging from about 600 to about 800; or from about 800 to about 1000; or from about 1000 to about 1200; or from about 1200 to about 1400; or from about 1400 to about 1600; or from about 1600 to about 1800, or from about 1800 to about 2000; or from about 2000 to about 2200.
  • D.P. degree of polymerization
  • suitable range of cellulose ether of the present invention can be varied from about 0.01 wt.% to about 5 wt.%; or from about 5 wt.% to about 10 wt.%; or from about 10 wt.% to about 15 wt.%; or from about 15 wt.% to about 20 wt.%; or from about 20 wt.% to about 25 wt.%; or from about 25 wt.% to about 30 wt.%; based on the total weight of the fluid suspension composition.
  • powdered cellulosic ether polymers including, but not limited to, methylhydroxypropylcellulose (MHPC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), carboxymethylhydroxyethylcellulose (CMHEC), hydroxyethylcellulose (HEC), hydrophobically modified hydroxy ethylcellulose (HMHEC), ethylhydroxy ethylcellulose (EHEC), hydrophobically modified ethylhydroxyethylcellulose (HMEHEC), methylhydroxyethylcellulose (MHEC), or combinations thereof; in aqueous based formulations can be significantly reduced using fluid suspension compositions of the present invention, compared to the conventional method involving direct addition of powdered cellulosic ethers.
  • MHPC methylhydroxypropylcellulose
  • HPC hydroxypropylcellulose
  • MC carboxymethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • CMC carboxymethylhydroxyethylcellulose
  • cellulosic ether polymers that contain sufficiently high polymer solids are found useful for the preparation of fluid polymer suspensions and can be effectively formulated in to an aqueous based compositions or used for post addition during the preparation of inorganic/metal slurries or pastes.
  • Suspensions of this type in general, comprise at least 10% by weight, preferably 15% by weight or higher, of a cellulose ether polymer selected from, but not limited to, the group of methylhydroxypropylcellulose (MHPC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), carboxymethylhydroxyethylcellulose (CMHEC), hydroxyethylcellulose (HEC), hydrophobically modified hydroxy ethylcellulose (HMHEC), ethylhydroxy ethylcellulose (EHEC), hydrophobically modified ethylhydroxyethylcellulose (HMEHEC), methylhydroxyethylcellulose (MHEC), or combinations thereof; in an aqueous liquid carrier.
  • a cellulose ether polymer selected from, but not limited to, the group of methylhydroxypropylcellulose (MHPC), hydroxypropylcellulose (HPC), methylcellulose (MC), carboxymethylcellulose (CMC), carboxymethylhydroxyethylcellulose (CM
  • the aqueous liquid carrier further contains dissolved or dispersed additives at sufficiently high concentrations to prevent the hydrophilic cellulose ether polymer from swelling substantially or dissolving in the aqueous medium, thus rendering it fluid, and allows the cellulose ether polymer particles to be properly dispersed and suspended, thus providing the stability.
  • small amounts, below 0.5% by weight of preservative is added to the composition to avoid microbial degradation and particle coagulation during storage.
  • insolubilizing agents such as inorganic salts.
  • inorganic salts may typically include but not limited to, sodium chloride, potassium chloride, sodium citrate, sodium sulfate, sodium formate, potassium phosphate, calcium formate, potassium formate, sodium acetate, potassium bicarbonate, sodium bicarbonate, diammonium phosphate, ammonium sulfate, or combinations thereof.
  • the concentration of inorganic salts must be adjusted such that the flocculation (or cloud) point, that is, the temperature at which a polymer precipitates or gels from solution to render a cloudy dispersion, is below room temperature.
  • the concentration of inorganic salts in the fluid polymer suspension must be sufficiently high to render the polymer insoluble in the salt water at the temperature at which the fluid polymer suspension is to be stored and used.
  • the inorganic salt concentration should be so high that swelling of the insolubilized polymer particles in the aqueous medium, if any, would occur only to a small degree.
  • inorganic salts in the fluidized polymer suspension is highly undesirable for some specialty applications which may include, but not limited to, washcoats, drilling fluids, specialty coatings, household products and agricultural products. It may interfere/influence with other additives such as metal particles within the formulation or, may lead to some unwanted chemical reactions with substrates or other materials/fluids it may come in contact with, during the end-user application. These inorganic salts also leave some residues on the substrates and not fully removable during calcination, which is highly undesirable for applications such as washcoats.
  • Present invention hence contemplates the use of a salt free insolubilizing agent for the preparation of stable fluid suspension composition, highly suitable for above mentioned applications.
  • the insolubilizing agent of the present invention is selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof.
  • suitable monosaccharides of the present invention include, but not limited to, glucose, dextrose, fructose, galactose, xylose, ribose, and combinations thereof;
  • suitable disaccharides of the present invention include, but not limited to, sucrose, lactose, maltose, lactulose, trehalose, and combinations thereof;
  • suitable polysaccharides of the present invention include, but not limited to, maltodextrin, starch, amylose, amylopectin, dextran, and combinations thereof.
  • the insolubilizing agent of the present invention is in the form of a powder, a liquid, or an aqueous solution thereof.
  • the insolubilizing agent of the present invention is an inverted sugar and suitable range of active content of the inverted sugar can be varied from about 65% to about 70%, or from about 70% to about 75%, or from about 75% to about 80%, or from about 80% to about 85%.
  • the insolubilizing agent of the present invention is an inverted sugar and suitable range of conversion rate of the inverted sugar can be varied from about 55% to about 60%, or from about 60% to about 65%, or from about 65% to about 70%, or from about 70% to about 75%.
  • suitable range of insolubilizing agent of the present invention can be varied from about 0.01 wt.% to about 5 wt.%; or from about 5 wt.% to about 10 wt.%; or from about 10 wt.% to about 15 wt.%; or from about 15 wt.% to about 20 wt.%; or from about 20 wt.% to about 25 wt.%; or from about 25 wt.% to about 30 wt.%; or from about 30 wt.% to about 35 wt.%; or from about 35 wt.% to about 40 wt.%; or from about 40 wt.% to about 45 wt.%; or from about 45 wt.% to about 50 wt.%; or from about 50 wt.% to about 55 wt.%; or from about 55 wt.% to about 60 wt.%; or from about 60 wt.% to about 65 w
  • the stabilizing agent of the present invention is selected from the group consisting of xanthan gum, sodium carboxymethyl cellulose, sodium alginate, bentonite clay, carrageenan, and combinations thereof.
  • suitable range of stabilizing agent of the present invention can be varied from about 0.01 wt.% to about 0.5 wt.%; or from about 0.5 wt.% to about 1 wt.%; or from about 1 wt.% to about 1.5 wt.%; or from about 1.5 wt.% to about 2 wt.%; or from about 2 wt.% to about 2.5 wt.%; or from about 2.5 wt.% to about 3 wt.%; or from about 3 wt.% to about 3.5 wt.%; or from about 3.5 wt.% to about 4 wt.%; or from about 4 wt.% to about 4.5 wt.%; or from about 4.5 wt.%; or from about 4.5 wt.%; or
  • the preservative of the present invention is selected from the group consisting of sodium benzoate, citric acid, benzyl alcohol, propylparaben, ethylparaben, butylparaben, methylparaben, benzylparaben, isobutylparaben, phenoxyethanol, ethanol, sorbic acid, benzoic acid, methylchloroisothiazolinone, methylisothiazolinone, methyl dibromoglutaronitrile, dehydroacetic acid, o-phenylphenol, l,2-benzisothiazoline-3-one, 5- chloro-2-methyl4-isothiazoline-3-one, benzyl bromoacetate, bicyclic oxazolidines, 4,4- dimethyloxazolidine, and combinations thereof.
  • suitable range of preservative of the present invention can be varied from about 0.01 wt.% to about 0.5 wt.%; or from about 0.5 wt.% to about 1 wt.%; or from about 1 wt.% to about 1.5 wt.%; or from about 1.5 wt.% to about 2 wt.%; or from about 2 wt.% to about 2.5 wt.%; or from about 2.5 wt.% to about 3 wt.%; or from about 3 wt.% to about 3.5 wt.%; or from about 3.5 wt.% to about 4 wt.%; or from about 4 wt.% to about 4.5 wt.%; or from about 4.5 wt.% to about 5 wt.%; based on the total weight of the fluid suspension composition.
  • the present application discloses a process for preparing an aqueous salt-free fluid suspension composition, wherein the process comprising the steps of:
  • step (b) adding about 0.01 wt.% to about 5 wt.% of least one stabilizing agent into the reaction container of step (a);
  • step (c) adding about 0.01 wt.% to about 5 wt.% of at least one preservative into the resultant of step (b); (d) adding about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent into the resultant of step (c) and continuing the agitation to achieve complete dissolution; and,
  • step (e) adding about 0.01 wt.% to about 30 wt.% of at least one cellulose ether into the resultant of step (d) and continuing the agitation till obtaining a homogenized fluid suspension composition.
  • the resulting polymer suspension composition of the present invention is typically fluid, pourable, and pumpable.
  • the suspension has a viscosity of less than 20,000 mPas one day after preparation, as measured with a Brookfield Model RVT viscometer at 20 rpm/20° C.
  • a preferred product, with total polymer solids of 15% or higher typically has a suspension viscosity of 20,000 mPas or less.
  • the fluid suspension composition of the present invention is further formulated into an aqueous system, for e.g., washcoats, mineral, inorganic, or metal powder slurries, etc.
  • the fluid suspension is diluted considerably, and the concentration of the additives becomes so low that the cellulose ether polymers will disperse and dissolve readily.
  • the suspension can disperse and dissolve in aqueous media at a much higher rate than the dry polymer, since the polymer particles in the suspension have been pre-wetted and, in many cases, are slightly swollen.
  • the instant invention allows a short mixing cycle of about 5-10 minutes rather than a 1 to 3 hour mixing period as required with convention cellulose ether polymer powder ingredients
  • productivity of manufacturing aqueous systems comprising (i) aqueous salt-free fluid suspension compositions of the present invention and (ii) other additives such as, but not limited to, precious metal particles, inorganic oxides, and acids, can be significantly increased.
  • the fluid suspension composition of the present invention is used for preparing aqueous based formulations that find applications in products including, but not limited to washcoats, drilling fluids, concrete, joint compound, mortar, adhesives, cosmetic products, personal care products, household products, agricultural products, paints, and paper coatings.
  • the present application discloses a thickening composition
  • a thickening composition comprising an aqueous salt-free fluid suspension composition comprising: (i) about 0.01 wt.% to about 30 wt.% of at least one cellulose ether, (ii) about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof, (iii) about 0.01 wt.% to about 5 wt.% of at least one stabilizing agent, (iv) about 0.01 wt.% to about 5 wt.% of at least one preservative, and (v) about 0.01 wt.% to about 70 wt.% of water.
  • the thickening composition of the present application is used in washcoats, drilling fluids, concrete, joint compound, mortar, adhesives, cosmetic products, personal care products, household products, agricultural products, paints, and paper coatings.
  • Another embodiment of the present invention provides a process for continuous preparation of aqueous slurry compositions which may include, but not limited to, washcoats, drilling fluids, concrete, joint compound, mortar, adhesives, cosmetic products, personal care products, household products, agricultural products, paints, or paper coatings, wherein the process involves the use of an aqueous salt-free fluid suspension composition comprising: (i) about 0.01 wt.% to about 30 wt.% of at least one cellulose ether, (ii) about 0.01 wt.% to about 90 wt.% of at least one insolubilizing agent selected from the group consisting of monosaccharide, disaccharide, polysaccharide, inverted sugar, and combinations thereof, (iii) about 0.01 wt.% to about 5 wt.% of at least one stabilizing agent, (iv) about 0.01 wt.% to about 5 wt.% of at least one preservative, and (v) about 0.01 wt.
  • the process for producing an aqueous slurry composition further comprises addition of ingredients comprising precious metals, acids, inorganic oxides, or combinations thereof.
  • Use of aqueous salt-free fluid suspension composition of the present invention further offers rapid viscosity adjustment and ease of handling during continuous preparation of the aqueous slurry compositions.
  • Another embodiment of the present invention further provides a washcoat formulation for applying a catalyst coating to a catalyst support.
  • the support carrier is usually in the form of a honeycomb which has passages for the flow of gas.
  • the honeycomb is used in catalytic converters for automobiles and in catalytic incinerators, which burn out pollutants in a stream of air.
  • a typical washcoat includes alumina and also the catalyst metal, so that the catalyst coating is applied in a single step.
  • the washcoat is intended especially for catalytic converters for automobiles or stationery.
  • the washcoat has a high solids content, an adjusted rheology profile, and it dries to a smooth, tightly-adhering coating without cracks.
  • the washcoat includes the catalyst metal, such as platinum, palladium, rhodium, or other catalytic active components.
  • the catalyst metals are dispersed on the alumina which leads to high dispersion of the metals and to high catalytic activity.
  • EXAMPLE 1 Preparation of fluid polymer suspension composition containing inorganic salt.
  • Fluid suspension composition according to above formulation was prepared by mixing the ingredients in following order to obtain a 100g sample:
  • Fluid suspension composition of Natrosol 250 MR was prepared according to above method and evaluated its stability in aqueous systems such as washcoats.
  • a washcoat sample was prepared using the fluid suspension composition of Example- 1 and investigated towards the viscosity development over time using an Anton Paar Rheometer MCR102 at various time intervals including (i) directly after preparation, (ii) after 3 days and (iii) after 5 days. It was observed that the fluid suspension composition of example- 1 showed unpredictable thickening behavior when interacted with the washcoat components. Due to the extreme low pH and catalytic components, the HEC (Natrosol 250 MR) of above formulation caused to react in a non-predictive way and failed to quickly provide a stable rheology value.
  • EXAMPLE 2 Reducing/eliminating the inorganic salt content of fluid polymer suspension
  • Fluid suspension compositions according to Examples 2(a)-2(k) of Table-1 were prepared by mixing the ingredients in following order to obtain a 100g sample:
  • Fluid suspension composition according to above formulation was prepared by mixing the ingredients in following order to obtain a 100g sample:
  • a two-component fluid suspension composition was prepared and tested for the stability.
  • Three 100ml plastic beakers equipped with screw cap were filled with 100ml of the final FPS formulation.
  • One beaker was stored in the fridge, one beaker was stored at room temperature and one beaker in a heating chamber at 40°C. All samples were stored for one month at the mentioned conditions and were regularly checked for separation or other changes. It found stable for over a month without any degradation or mold growth however, the composition showed a little syneresis during storage.
  • EXAMPLE 4 Preparation of stable fluid suspension composition.
  • Fluid suspension composition according to above formulation was prepared by mixing the ingredients in following order to obtain a 100g sample:
  • a fluid suspension composition was prepared and tested for the stability.
  • Three 100ml plastic beaker equipped with screw cap were filled with 100ml of the final FPS formulation.
  • One beaker was stored in the fridge, one beaker was stored at room temperature and one in a heating chamber at 40°C. All samples were stored for one month at the mentioned conditions and were regularly checked for separation or other changes. None of the samples showed any deviation during the one-month period. The composition showed better stability on storage.
  • EXAMPLE 5 Trials with other cellulose ethers:
  • Fluid suspension compositions of Example 5(a) - 5(c) according to Table-2 were prepared by mixing the ingredients in following order to obtain a 100g sample: 1. 19.7g of purified water was charged in a reaction container equipped with an impeller stirrer.
  • Fluid suspension compositions of Benecel E10M, Culminal MHPC 724, and Klucel HXF were obtained according to above method. After preparation, the fluidized polymer suspension composition samples were investigated towards the flow behavior by pouring it out of the preparation vessel into a graded cylinder. The visual inspection gave insight onto homogeneity and viscosity. The graduated cylinder was sealed with a cling foil and put aside to check for separation and stability for one week.
  • Example 5(a) works, stable, but a little thicker than Example 4
  • Example 5(b) works, stable, thicker than Example 4, thinner than Example 5(a)
  • Example 5(c) works, stable, but a little thicker than Example 4
  • EXAMPLE 6 Dissolution behavior: [0093] Dissolution behavior of fluidized polymer suspension based on MHPC and typical dry cellulose ether powders such as (i) Natrosol 250MR HEC, and (ii) Culminal MHEC 6000PR, suspended in an aqueous solution at ambient temperature and at varying pH levels (pH 3, pH 7 and pH 11) were measured. Brookfield R/S+ rheometer using V80/40 vane spindle at 400 rpm was used to measure the torque development over time. All viscosity values were normalized towards a percentage scale to have the direct comparison of the viscosity development.
  • FIG. 1-3 illustrate the dissolution behavior as an indicative of dissolution time measured at various pH levels such as pH 3, pH 7 and pH 11 for a fluidized polymer suspension based on MHPC relative to a typical dry cellulose ether powder (Natrosol 250MR HEC) suspended in an aqueous solution at ambient temperature.
  • the magnitude of increase in dissolution rate with the fluid polymer suspension composition is striking. It takes a typical fluid polymer suspension composition less than five minutes to develop more than 95% of the ultimate solution viscosity, while the conventional dry polymer powder takes more than 40 minutes under the same conditions.
  • FIG. 1-3 illustrate the dissolution behavior as an indicative of dissolution time measured at various pH levels such as pH 3, pH 7 and pH 11 for a fluidized polymer suspension based on MHPC relative to a typical dry cellulose ether powder (Natrosol 250MR HEC) suspended in an aqueous solution at ambient temperature.
  • the magnitude of increase in dissolution rate with the fluid polymer suspension composition is striking. It takes a typical fluid polymer suspension composition
  • 4-5 illustrate the dissolution behavior as an indicative of dissolution time measured at various pH levels such as pH 3, pH 7 for a fluidized polymer suspension based on MHPC relative to a typical dry cellulose ether powder (Culminal MHEC 6000PR) suspended in an aqueous solution at ambient temperature.
  • the magnitude of increase in dissolution rate with the fluid polymer suspension composition is striking in this example as well. It takes a typical fluid polymer suspension composition less than five minutes to develop more than 95% of the ultimate solution viscosity, while the conventional dry polymer powder takes more than 100 minutes under the same conditions.

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Abstract

La présente demande concerne une composition de suspension fluide stable, sans sel, à base aqueuse comprenant : (i) environ 0,01 % en poids à environ 30 % en poids d'au moins un éther de cellulose, (ii) environ 0,01 % en poids à environ 90 % en poids d'au moins un agent d'insolubilisation choisi dans le groupe constitué par un monosaccharide, un disaccharide, un polysaccharide, un sucre inversé et des combinaisons de ceux-ci, (iii) environ 0,01 % en poids à environ 5 % en poids d'au moins un agent stabilisant, (iv) environ 0,01 % en poids à environ 5 % en poids d'au moins un conservateur, et (v) environ 0,01 % en poids à environ 70 % en poids d'eau.
EP23850850.1A 2022-08-01 2023-07-25 Compositions de suspension fluide stable sans sel aqueux et leur procédé de préparation Pending EP4565646A2 (fr)

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