EP1979418A1 - Utilisation de dispersants pour concentrer des matieres minerales dans l'eau, dispersions obtenues et leurs utilisations - Google Patents

Utilisation de dispersants pour concentrer des matieres minerales dans l'eau, dispersions obtenues et leurs utilisations

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Publication number
EP1979418A1
EP1979418A1 EP06831756A EP06831756A EP1979418A1 EP 1979418 A1 EP1979418 A1 EP 1979418A1 EP 06831756 A EP06831756 A EP 06831756A EP 06831756 A EP06831756 A EP 06831756A EP 1979418 A1 EP1979418 A1 EP 1979418A1
Authority
EP
European Patent Office
Prior art keywords
mineral
mineral matter
acrylic acid
homopolymer
dry weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP06831756A
Other languages
German (de)
English (en)
French (fr)
Inventor
Christian Jacquemet
Jacques Mongoin
Jean-Marc Suau
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coatex SAS
Original Assignee
Coatex SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Coatex SAS filed Critical Coatex SAS
Publication of EP1979418A1 publication Critical patent/EP1979418A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/06—Selection or use of additives to aid disintegrating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • C09C1/022—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C09C1/42—Clays
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/64—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/38—Coatings with pigments characterised by the pigments
    • D21H19/385—Oxides, hydroxides or carbonates
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • D21H19/36—Coatings with pigments
    • D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/56—Macromolecular organic compounds or oligomers thereof obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H19/58—Polymers or oligomers of diolefins, aromatic vinyl monomers or unsaturated acids or derivatives thereof

Definitions

  • the invention relates first of all to the use of new dispersing agents for concentrating mineral matter in water.
  • aqueous dispersions of mineral matter then obtained as well as their uses in aqueous formulations containing mineral materials such as calcium carbonate, and in particular in the fields of paper and more particularly in the context of the manufacture of the sheet. of paper and coating the paper sheet, paint, plastic and cosmetics such as in particular in the manufacture of dental pasta.
  • aqueous dispersions and suspensions of mineral matter such as in particular calcium carbonate
  • dispersion agents and / or grinding aid based on homopolymers and and / or acrylic copolymers in order to maintain said mineral matter in suspension in water at high solids concentrations and stably in time.
  • a dispersing agent being introduced between step a) and step b), and / or during step b), and / or during and after step b).
  • the Applicant may refer to such a process through the expression "low-solids dry milling process without dispersing agent and high solids concentration in the presence of dispersant".
  • Patent EP 0 850 685 teaches another solution which consists in the use of copolymers of acrylic acid and maleic acid, having a molar ratio between these two units of between 2: 1 and 10: 1, and an average molecular weight of between 1,000 and 100,000 Daltons.
  • aqueous dispersions of mineral particles such as, in particular, carbonate of calcium
  • having a high solids content greater than 65% by weight of mineral matter relative to the total weight of the dispersion
  • an instant Brookfield TM viscosity measured at 100 rpm lower than 5000 mPas in the course of a step of mechanical and / or thermal concentration, following a grinding step with a low dry matter concentration (less than 40% by weight of mineral matter relative to the total weight of the dispersion), in an aqueous medium and without the use of dispersant and / or grinding aid agent, which none of the documents of the prior art proposed, with the exception of the documents WO 01/048 093 and EP 0 850 685.
  • the present invention allows the skilled person to use homopolymers of acrylic acid without any restriction on them.
  • the use according to the invention of homopolymers of acrylic acid in combination with a fluorinated mineral compound allows the skilled person to disperse calcium carbonate according to the low-grinding process. dry extract without dispersing agent and then high solids concentration concentration in the presence of dispersing agent.
  • the present invention enables the person skilled in the art to obtain, by optimization of the pair formed by the homopolymer of acrylic acid and of the fluorinated mineral compound, solutions which surprisingly prove to be even more efficient than those proposed in the documents WO 01/04893 and EP 0 850 685; some of the solutions described in the present Application make it possible for the skilled person to obtain very high solids (greater than 70% by weight of mineral matter relative to the total weight of the dispersion) and an immediate Brookfield® viscosity. measured at 100 rpm very low (less than 500 mPa.s and sometimes even less than 250 mPa.s), which is not disclosed in both WO01 / 048 093 and EP 0 850 685.
  • the present invention is therefore based on the use of dispersing agents in a process for producing an aqueous dispersion of mineral matter, comprising the steps of:
  • step b) concentration of the aqueous suspension of mineral matter obtained during step a), by mechanical and / or thermal means, in order to obtain an aqueous dispersion of mineral matter whose concentration in dry weight of mineral matter is at least 65% of the total weight of said dispersion,
  • step a) and step b) at least one dispersing agent is introduced between step a) and step b), and / or during step b), and / or during and after step b),
  • Brookfield TM immediately measured at 100 rpm less than 5000 mPa.s, mineral particles such as calcium carbonate in particular, resulting from the low solids dry milling process without dispersing agent and high solids concentration concentration in the presence of dispersing agent.
  • This solution is based on the use of dispersing agents in a process for producing an aqueous dispersion of mineral matter, comprising the steps of:
  • step a) concentration of the aqueous suspension of mineral matter obtained in step a), by mechanical and / or thermal means, in order to obtain a concentration in dry weight of mineral matter of at least 65% of the total weight of said dispersion,
  • step a) and step b) at least one dispersing agent is introduced between step a) and step b), and / or during step b), and / or during and after step b),
  • step b) The mechanical and thermal concentration means used during step b) are chosen from those well known to those skilled in the art.
  • step a) and step b) may also use, at the time of his choice-that is to say between step a) and step b), and / or during step b), and / or during and after step b) - any other dispersing agent of the prior art, in order to optimize the characteristics of the final dispersion of mineral matter that it wishes to obtain.
  • the use of dispersing agents according to the invention is characterized in that the aqueous suspension of mineral material obtained during step a) has a dry weight concentration of mineral matter preferably less than 35%, more preferably less than 30%, and in that the aqueous dispersion of mineral matter obtained during step b) has a dry weight concentration of mineral matter that is preferably greater than 68%, more preferably greater than 70%.
  • aqueous dispersion of mineral material obtained immediately after step b) has a Brookfield TM viscosity measured at 100 rpm less than 5000 mPa.s, preferably less than 2000 mPa.s, very preferably less than 1000 mPa.s, and extremely preferably less than 500 mPa.s.
  • dispersing agents are also characterized in that the mineral materials are chosen from natural or synthetic calcium carbonate, dolomites, kaolin, talc, cement, gypsum, lime, magnesia, titanium dioxide, satin white, aluminum trioxide or aluminum trihydroxide, silicas, mica and the mixture of these fillers together, such as talc-calcium carbonate mixtures, calcium carbonate -kaolin, or mixtures of calcium carbonate with aluminum trihydroxide or aluminum trioxide, or mixtures with synthetic or natural fibers or the co-structures of minerals such as talc-carbonate co-structures calcium or talc-titanium dioxide, or mixtures thereof.
  • the mineral materials are chosen from natural or synthetic calcium carbonate, dolomites, kaolin, talc, cement, gypsum, lime, magnesia, titanium dioxide, satin white, aluminum trioxide or aluminum trihydroxide, silicas, mica and the mixture of these fillers together, such as talc-calcium carbonate mixtures, calcium
  • they are chosen from natural or synthetic calcium carbonates or talc or kaolin or their mixtures
  • dispersing agents according to the invention is also characterized in that the fluorinated mineral compound on the one hand and the homopolymer of acrylic acid on the other hand are introduced simultaneously, or in that first the fluorinated mineral compound and then the homopolymer of acrylic acid, or firstly the homopolymer of acrylic acid and then the fluorinated mineral compound.
  • dispersing agents according to the invention is also characterized in that the fluorinated mineral compound and the homopolymer of acrylic acid are introduced in the form of an aqueous suspension and / or of an aqueous solution when they are introduced simultaneously.
  • dispersing agents according to the invention is also characterized in that the fluorinated mineral compound is introduced in powder form and / or in the form of an aqueous suspension and / or in the form of an aqueous solution, and the homopolymer of acrylic acid is introduced in the form of an aqueous solution when these two compounds are introduced one after the other and this, regardless of the order of introduction.
  • dispersing agents according to the invention is also characterized in that it is used between 0.1% and 3.0%, and preferably between 0.5% and 1.5%, by weight. dry with respect to the dry weight of mineral matter, at least one homopolymer of acrylic acid.
  • dispersing agents according to the invention is also characterized in that it is implemented between 0.01% and 0.5%, and preferably between 0.05% and 0.25%, by dry weight. relative to the dry weight of mineral matter, at least one fluorinated mineral compound.
  • the use of dispersing agents according to the invention is also characterized in that the fluorinated mineral compound is chosen from the compounds NaF, NaHF 2 , H 2 SiF 6 , HKF 2 , FeF 2 , PbF 2 , HNH 4 F 2 and their mixtures, preferably among the compounds NaF, H 2 SiF 6 , HKF 2 , and mixtures thereof, and in that it is preferably the compound NaF.
  • the fluorinated mineral compound is chosen from the compounds NaF, NaHF 2 , H 2 SiF 6 , HKF 2 , FeF 2 , PbF 2 , HNH 4 F 2 and their mixtures, preferably among the compounds NaF, H 2 SiF 6 , HKF 2 , and mixtures thereof, and in that it is preferably the compound NaF.
  • dispersing agents according to the invention is also characterized in that the homopolymer of the acrylic acid used is neutralized, totally or partially, with a neutralization agent chosen from hydroxides and / or calcium oxides. , magnesium, hydroxides of sodium, potassium, or ammonia, or mixtures thereof, preferably with a neutralizing agent selected from sodium hydroxide, ammonia, or mixtures thereof, very preferably with a neutralization agent which is ammonia.
  • dispersing agents according to the invention is also characterized in that the homopolymer of the acrylic acid employed has an average molecular mass of between 1,000 and 150,000 Daltons, preferably between 5,000 and 100,000 Daltons, and more preferably between 15,000 and 80,000 Daltons.
  • dispersing agents according to the invention is also characterized in that the homopolymer of acrylic acid has a degree of neutralization, expressed as a molar percentage of neutralized acid sites, of between 10 and 100, preferably between 50 and 100. and 100, and more preferably between 70 and 100.
  • Another object of the invention resides in the aqueous dispersions of mineral materials obtained by use according to the invention, in a manufacturing process, comprising the steps of: (a) preparation of an aqueous suspension of mineral material by grinding said inorganic materials without dispersing agent and / or grinding aid agent, said suspension having a concentration by dry weight of mineral matter less than or equal to 40% of its weight total,
  • step a) concentration of the aqueous suspension of mineral matter obtained during step a), by mechanical and / or thermal means, in order to obtain a concentration by dry weight of mineral matter of at least 65% of the total weight of said dispersion,
  • Another subject of the invention is based on aqueous dispersions of mineral matter, characterized in that they contain:
  • aqueous dispersions of mineral matter are also characterized in that they have a concentration in dry weight of mineral matter, preferably greater than 68%, more preferably greater than 70%.
  • aqueous dispersions of mineral matter are also characterized in that the mineral materials are chosen from natural or synthetic calcium carbonate, dolomites, kaolin, talc, cement, gypsum, lime, magnesia, carbon dioxide and the like. titanium, satin white, aluminum trioxide or aluminum trihydroxide, silicas, mica and the mixture of these fillers together, such as talc-calcium carbonate, calcium carbonate-kaolin mixtures, or mixtures of calcium carbonate with aluminum trihydroxide or aluminum trioxide, or mixtures with synthetic or natural fibers or co-polymers mineral structures such as talc-calcium carbonate or talc-titanium co-structures, or mixtures thereof.
  • the mineral materials are chosen from natural or synthetic calcium carbonate, dolomites, kaolin, talc, cement, gypsum, lime, magnesia, carbon dioxide and the like.
  • they are chosen from natural or synthetic calcium carbonates or talc or kaolin or their mixtures. Very preferably, they are chosen from natural or synthetic calcium carbonates or mixtures thereof.
  • aqueous dispersions of mineral matter are also characterized in that they contain between 0.1% and 3.0%, preferably between 0.5% and 1.5%, by dry weight relative to the dry weight of mineral matter, at least one homopolymer of acrylic acid.
  • aqueous dispersions of mineral matter are also characterized in that they contain between 0.01% and 0.5%, and preferably between 0.05% and 0.25%, by dry weight relative to the dry weight of mineral matter. at least one fluorinated mineral compound.
  • aqueous dispersions of mineral matter are also characterized in that the fluorinated mineral compound is chosen from the compounds NaF, NaHF 2 , H 2 SiF 6 , HKF 2 , FeF 2 , PbF 2 , HNH 4 F 2 and mixtures thereof, preferably from the compounds NaF, H 2 SiF 6 , HKF 2 , and mixtures thereof, and in that it is preferably the NaF compound.
  • the fluorinated mineral compound is chosen from the compounds NaF, NaHF 2 , H 2 SiF 6 , HKF 2 , FeF 2 , PbF 2 , HNH 4 F 2 and mixtures thereof, preferably from the compounds NaF, H 2 SiF 6 , HKF 2 , and mixtures thereof, and in that it is preferably the NaF compound.
  • aqueous dispersions of mineral matter are also characterized in that the homopolymer of the acrylic acid used is neutralized, totally or partially, with a neutralization agent chosen from hydroxides and / or oxides of calcium, magnesium, hydroxides of sodium, potassium, or ammonia, or mixtures thereof, preferably with a neutralizing agent chosen from sodium hydroxide, ammonia, or mixtures thereof, very preferably with a neutralizing agent which is ammonia .
  • a neutralization agent chosen from hydroxides and / or oxides of calcium, magnesium, hydroxides of sodium, potassium, or ammonia, or mixtures thereof, preferably with a neutralizing agent chosen from sodium hydroxide, ammonia, or mixtures thereof, very preferably with a neutralizing agent which is ammonia .
  • aqueous dispersions of mineral matter are also characterized in that the homopolymer of the acrylic acid used, has an average molecular mass of between 1000 and 150 000 Daltons, preferably between 5000 and 100 000 Daltons and more preferably between 15 000 and 80,000 Daltons.
  • These aqueous dispersions of mineral matter are also characterized in that the homopolymer of acrylic acid, has a degree of neutralization, expressed in molar percentage of neutralized acid sites, between 10 and 100, preferably between 50 and 100, and more preferably between 70 and 100.
  • Another object of the invention resides in the use of these aqueous dispersions in the fields of the manufacture of aqueous formulations containing mineral substances, in particular in the field of paper, and more particularly in the manufacture of the paper sheet and in the manufacture of coating coatings intended for the production of a sheet of coated paper, in the plastics and paint sectors, as well as in cosmetics and more particularly in the manufacture of dental pastes.
  • step a) concentration of the aqueous suspension of calcium carbonate thus obtained during step a) by means of a thermal evaporator, in order to obtain the highest concentration in dry weight of mineral matter,
  • a dispersing agent according to the invention in the form of a combination: at least one homopolymer of acrylic acid, totally or partially neutralized,
  • Brookfield TM viscosity at 100 rpm immediately after step b) was determined for each aqueous dispersion of mineral material and according to the methods well known to those skilled in the art. 25 ° C, noted ⁇ 100 to .
  • This test illustrates the invention and uses, relative to the dry weight of calcium carbonate: - 0.75% by dry weight of a homopolymer of acrylic acid, 70 mol% of the acid sites are neutralized by sodium hydroxide and weight molecular M w equal to 13,300 Daltons, and having a viscosity index (as measured according to the method described in WO 01/048 093) equal to 0.075, - and 0, 10% by dry weight of sodium fluoride.
  • This test illustrates the invention and uses, relative to the dry weight of calcium carbonate: - 0.75% by dry weight of a homopolymer of acrylic acid completely neutralized with ammonia and of molecular weight M w equal to 10,000 Daltons, and having a viscosity number (as measured according to the method described in WO 01/04893) equal to 0.07,
  • This test illustrates the invention and uses, relative to the dry weight of calcium carbonate: - 0.80% by dry weight of a homopolymer of acrylic acid, 40 mol% of the acid sites are neutralized by sodium hydroxide, with a molecular weight M w equal to 10,000 Daltons, and having a viscosity number (as measured according to the method described in WO 01/04893) equal to 0.07, - and 0, 10 % by dry weight of sodium fluoride.
  • This test illustrates the invention and uses, relative to the dry weight of calcium carbonate: - 0.70% by dry weight of a homopolymer of acrylic acid, of which 80 mol% of the acidic sites are neutralized by sodium hydroxide and molecular weight M w equal to 10,000 Daltons, and having a viscosity index (as measured according to the method described in WO 01/048 093) equal to 0.07, - 0.10 and % by dry weight of sodium fluoride.
  • This test illustrates the invention and uses, relative to the dry weight of calcium carbonate: - 0.70% by dry weight of a homopolymer of acrylic acid, 60 mol% of the acid sites are neutralized by sodium hydroxide and molecular weight M w equal to 10,000 Daltons, and having a viscosity index (as measured according to the method described in WO 01/048 093) equal to 0.07, - 0.10 and % by dry weight of sodium fluoride. Test n ° 7
  • Test No. 16 This test illustrates the invention and uses, relative to the dry weight of calcium carbonate:
  • Test No. 17 This test illustrates the invention and uses, relative to the dry weight of calcium carbonate:
  • Table 1 characteristics of the dispersants according to the invention and ES and ⁇ ioo values for the dispersions obtained according to the invention.
  • Neutral rate. 1 (%) denotes the degree of neutralization of each homopolymer, expressed as molar percentage of neutralized acid sites
  • amount 2 denotes the amount of homopolymer used, expressed as a percentage by dry weight of said polymer relative to the total dry weight of mineral matter
  • amount 3 represents the quantity of fluorinated mineral compound used, expressed as a percentage by dry weight of said fluorinated mineral compound relative to the total dry weight of mineral matter
  • - ES denotes the dry extract expressed as a percentage by dry weight of mineral matter relative to the total weight of each dispersion.
  • this table demonstrates that the use of dispersants according to the invention makes it possible, in the process described above, to obtain aqueous dispersions of calcium carbonate with concentrations by dry weight of mineral matter greater than 65%, and an instant Brookfield TM viscosity measured at 100 rpm less than 5000 mPa.s.
  • Test No. 18 This test illustrates the prior art and uses 0.75% by dry weight, relative to the dry weight of calcium carbonate, of a homopolymer of acrylic acid totally neutralized with sodium hydroxide. and of molecular weight equal to 14,000 Daltons.
  • Test n ° 19 This test illustrates the prior art and implements 0.75% by dry weight, relative to the dry weight of calcium carbonate, of a homopolymer of acrylic acid completely neutralized by sodium hydroxide and of molecular weight. equal to 12,000 Daltons.
  • This test illustrates the prior art and implements 0.75% by dry weight, relative to the dry weight of calcium carbonate, of a homopolymer of acrylic acid completely neutralized with ammonia and of molecular weight equal to 10,000 Daltons.
  • This test illustrates the prior art and uses 0.80% by dry weight, relative to the dry weight of calcium carbonate, of a homopolymer of acrylic acid completely neutralized with ammonia and of molecular weight equal to 10,000 Daltons.
  • This test illustrates the prior art and uses 0.85% by dry weight, relative to the dry weight of calcium carbonate, of a homopolymer of acrylic acid completely neutralized with ammonia and of molecular weight equal to 10,000 Daltons.
  • Table 2 Characteristics of the dispersants according to the prior art and ES values and ⁇ 100 for the dispersions obtained. In this table :
  • amount 2 denotes the amount of homopolymer used, expressed as a percentage by dry weight of said polymer relative to the total dry weight of mineral matter, ⁇ 10 0 t0 denotes the Brookfield TM viscosity measured at 100 rpm immediately after step b ), and noted ⁇ ⁇ o t0 ,
  • - ES denotes the dry extract expressed as a percentage by dry weight of mineral matter relative to the total weight of each dispersion.
  • This test illustrates the prior art and uses, relative to the dry weight of calcium carbonate, 0.75% by dry weight of a homopolymer of acrylic acid totally. neutralized with sodium hydroxide, and with a molecular weight M w equal to 50,000 Daltons, and having a viscosity number (as measured according to the method described in WO 01/04893) equal to 0.8.
  • Brookfield TM viscosity values measured at t 0, at 25 ° C., and at a rotational speed of 100 rpm (in mPa.s) denoted by ⁇ 10 0 t 0 , and the values of the dry extract (in percentage by dry weight of mineral matter relative to the total weight of the dispersion obtained) noted ES, are indicated in Table 3.
  • Table 3 also shows the results obtained for tests 2, 7 and 14.
  • Table 3 characteristics of the dispersants according to the invention and ES values and ⁇ 10 O 10 for the dispersions obtained according to the invention.
  • homopolymer denotes a homopolymer of acrylic acid
  • copolymer denotes a copolymer of acrylic acid and of maleic anhydride (in a 3: 1 molar mixture) and of molecular weight
  • amount 2 denotes the amount of homopolymer or copolymer used, expressed as a percentage by dry weight of said polymer relative to the total dry weight of mineral matter,
  • amount 3 represents the amount of fluorinated mineral compound used, expressed as a percentage by dry weight of said fluorinated mineral compound relative to the total dry weight of mineral matter, - ⁇ 10 Te 10 denotes the Brookfield TM viscosity measured at 100 rpm immediately after step b), and denoted ⁇ jo û t0,
  • - ES denotes the dry extract expressed as a percentage by dry weight of mineral matter relative to the total weight of each dispersion.
  • step a) concentration of the aqueous suspension of calcium carbonate thus obtained during step a) by means of a thermal evaporator, in order to obtain the highest concentration in dry weight of mineral matter,
  • a dispersing agent according to the invention has been used in the form of a combination of: at least one homopolymer of acrylic acid, totally or partially neutralized, and at least one fluorinated mineral compound.
  • Brookfield TM viscosity was determined for each aqueous dispersion of mineral material and according to methods well known to those skilled in the art at 100 rpm immediately after step b), at 25 ° C. , denoted ⁇ 10 o t0 .
  • Test No. 25 This test illustrates the invention and uses, relative to the dry weight of calcium carbonate:
  • step a) - 0, 10% by dry weight of NaHF 2 , introduced between step a) and step b),
  • Table 4 characteristics of the dispersants according to the invention and ES values and ⁇ 10 10 for the dispersions obtained according to the invention.
  • Table 4 lists the abbreviations in Table 1, their meaning having been given previously.
  • this table demonstrates that the use of dispersants according to the invention makes it possible, in the process described above, to obtain aqueous dispersions of calcium carbonate with concentrations by dry weight of mineral matter greater than 65%, and an instant Brookfield TM viscosity measured at 100 rpm less than 5000 mPa.s.
  • step a) concentration of the aqueous suspension of calcium carbonate thus obtained during step a) by means of a thermal evaporator, in order to obtain the highest concentration in dry weight of mineral matter,
  • RAFT controlled radical polymerization method
  • the Applicant states that all the homopolymers of the acrylic acid used in tests Nos. 1 to 26 were obtained by conventional polymerization methods.
  • Table 5 Characteristics of the dispersant according to the invention and ES value and ⁇ 10 10 for the dispersion obtained according to the invention.
  • Reading from Table 5 demonstrates that the use of the dispersant according to the invention makes it possible to disperse efficiently and at concentrations by dry weight of mineral matter greater than 65% of the total weight of said dispersion, an initial suspension of calcium carbonate which had was milled without a dispersing agent or grinding aid agent at a solids concentration of less than 40% of the total weight of said suspension.
  • this table demonstrates that the use of the dispersant according to the invention makes it possible, in the process described above, to obtain aqueous dispersions of calcium carbonate with concentrations by dry weight of mineral matter greater than 65%, and an instant Brookfield TM viscosity measured at 100 rpm less than 5000 mPa.s.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paper (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Cosmetics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Paints Or Removers (AREA)
EP06831756A 2005-12-20 2006-12-13 Utilisation de dispersants pour concentrer des matieres minerales dans l'eau, dispersions obtenues et leurs utilisations Withdrawn EP1979418A1 (fr)

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FR0512928A FR2894846B1 (fr) 2005-12-20 2005-12-20 Utilisation de dispersants pour concentrer des matieres minerales dans l'eau, dispersions obtenues et leurs utilisations.
PCT/IB2006/003681 WO2007072168A1 (fr) 2005-12-20 2006-12-13 Utilisation de dispersants pour concentrer des matieres minerales dans l'eau, dispersions obtenues et leurs utilisations

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FR2899825B1 (fr) * 2006-04-14 2010-08-13 Coatex Sas Dispersion aqueuse de carbonate de calcium precipite a partir d'au moins un agent dispersant contenant un compose porteur d'ion fluorure.
EP2194103A1 (en) 2008-12-04 2010-06-09 Omya Development Ag Process for manufacturing calcium carbonate materials having a particle surface with improved adsorption properties
FR2940141B1 (fr) 2008-12-19 2010-12-17 Coatex Sas Utilisation de polymeres acryliques neutralises par le lithium comme agents dispersants ou d'aide au broyage en milieu aqueux de matieres minerales
EP2199348A1 (en) 2008-12-19 2010-06-23 Omya Development AG Process for manufacturing aqueous suspensions of mineral materials or dried mineral materials, the obtained products, as well as uses thereof
JP2011105853A (ja) * 2009-11-17 2011-06-02 Fimatec Ltd 湿式粉砕助剤及び微粒重質炭酸カルシウム分散体
PT2390284E (pt) 2010-05-28 2012-06-01 Omya Development Ag Processo de fabrico de suspensões com elevado teor de sólidos de materiais minerais
PT2455429E (pt) 2010-11-19 2013-11-07 Omya Int Ag Processo de preparação de suspensões aquosas de materiais minerais por meio de aminas, em combinação com polímeros vinilcarboxílicos
FR2967593B1 (fr) 2010-11-19 2012-12-28 Coatex Sas Utilisation d'amines en combinaison avec des polymeres acryliques dans la fabrication de suspensions aqueuses de matieres minerales
JP2014505753A (ja) 2010-12-17 2014-03-06 ビーエーエスエフ ソシエタス・ヨーロピア 安定なポリアクリル酸、その製造およびその使用
EP2628775A1 (en) * 2012-02-17 2013-08-21 Omya Development AG Mineral material powder with high dispersion ability and use of said mineral material powder
EP2712895B1 (en) 2012-09-26 2016-05-18 Omya International AG Rheologically stable aqueous mineral material suspensions comprising organic polymers having reduced volatile organic compound (voc) content
US9951196B2 (en) * 2012-10-24 2018-04-24 J.M. Huber Corporation Cationic polyoxometalate-coated alumina trihydrate dispersants
CN106320065B (zh) * 2015-06-26 2018-03-27 池州学院 一种高固含量滑石粉和重质碳酸钙粉浆体的制备方法
CN106835828B (zh) * 2016-12-25 2018-06-01 安徽鑫雅包装制品有限公司 一种低粘度高分散型造纸滑石粉的制备方法
CN110862238B (zh) * 2019-11-28 2022-03-25 中建商品混凝土有限公司 一种搅拌站废浆湿磨用分散剂

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RU2008129817A (ru) 2010-01-27
CN101341217A (zh) 2009-01-07
TW200727975A (en) 2007-08-01
FR2894846A1 (fr) 2007-06-22
FR2894846B1 (fr) 2008-02-01
AR058547A1 (es) 2008-02-13
JP2009520096A (ja) 2009-05-21
CA2629622A1 (fr) 2007-06-28
KR20080078672A (ko) 2008-08-27
NO20082981L (no) 2008-07-24
US20090111906A1 (en) 2009-04-30

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