EP2387601A1 - Utilisation de polymeres acryliques peigne avec des groupes hydrophobes comme agents de couplage dans un procede de broyage de matieres minerales avec des liants - Google Patents
Utilisation de polymeres acryliques peigne avec des groupes hydrophobes comme agents de couplage dans un procede de broyage de matieres minerales avec des liantsInfo
- Publication number
- EP2387601A1 EP2387601A1 EP10701720A EP10701720A EP2387601A1 EP 2387601 A1 EP2387601 A1 EP 2387601A1 EP 10701720 A EP10701720 A EP 10701720A EP 10701720 A EP10701720 A EP 10701720A EP 2387601 A1 EP2387601 A1 EP 2387601A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- monomer
- use according
- acrylic
- mixtures
- coupling agent
- 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- Withdrawn
Links
Classifications
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- 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
- 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
- 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
- C09C3/10—Treatment with macromolecular organic compounds
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Definitions
- Binders and minerals are among the main constituents of paper.
- the former in the form of dispersions or aqueous latex suspensions, provide the necessary cohesion to all the constituents involved in the manufacture of said paper.
- the latter such as calcium carbonate, make it possible to improve the quality of the paper sheet, in particular as regards its optical properties.
- hybrid particles or “self-binding” particles were born a few years ago: they are solid, individual particles in which mineral particles and latex particles are intimately bound. The internal cohesion forces are such that the particles obtained have excellent mechanical stability, and can be used directly in the manufacture of paper.
- the processes for producing such particles involve at least one step of grinding mineral materials in the presence of binders. Grinding is understood to mean an operation leading to a reduction in particle sizes: the size of the hybrid particles formed is smaller than that of the initial mineral particles.
- WO 2006 008657 describes a process for co-grinding in an aqueous medium of inorganic materials in the presence of binders. The self-binding character is measured from a crushing test performed on specimens made from the solid particles resulting from the co-grinding step.
- the document WO 2006 128814 looks at the impact of such hybrid particles on the final properties of the paper sheet: it attests, in particular, an improvement in the optical properties of the sheet, such as its opacity. It describes the manufacture of these particles through a grinding process in calcium carbonate water in the presence of binders, in particular with Polygen TM WE 4 (in 3 of the 4 tests). On the other hand, none of the resulting aqueous suspensions has a solids content in mineral matter greater than 30% of its weight.
- WO 2008 139292 discloses a method implementing a step of grinding a binder in the presence of a mineral material, followed by the addition of an inverse emulsion; the tests illustrate the implementation of Polygen TM WE 4, to grind at a concentration of 20% dry matter a mixture of calcium carbonate with binder, the product obtained being concentrated at 40%.
- step a) at least one step of grinding in an aqueous medium of at least one latex and at least one mineral material, b) optionally at least one suspension concentration stage resulting from step a), with possibly at least one a dispersing agent, c) optionally at least one step of drying the suspension resulting from step a) or b),
- At least one other monomer which is preferably an acrylic ester and very preferably ethyl acrylate is an unsaturated amide and very preferably acrylamide.
- the coupling agent according to the invention it is possible to obtain hybrid particles having a cohesive character which is just as marked as for the prior art (Polygen TM WE A), as illustrated by measurements of the quantity of material organic (TOC) present in the aqueous phase.
- TOC material organic
- the Applicant estimates that the lower the TOC values, the better the cohesive forces within the hybrid particles: in the aqueous phase, only a small amount of latex, tensio- actives (which serve to stabilize the latex) and coupling agent.
- the water resulting from the reconcentration process can thus be reused, which constitutes another advantage resulting from the present invention.
- the coupling agent according to the invention is used in doses identical to that in which the Polygen of the prior art was used. It is then demonstrated that aqueous suspensions of self-binding particles having a dry matter content and a rheological behavior similar to those obtained with Polygen are obtained.
- the present invention offers the skilled person an alternative to the single product revealed by the prior art, which contributes to enriching the state of the art and gives greater freedom to the practitioner.
- the coupling agent used during the grinding step a) makes it possible to directly reach a very high solids content for the aqueous suspension of hybrid particles manufactured: the concentration step is no longer necessary.
- a first object of the invention is the use, as a coupling agent, in a process for manufacturing self-binding particles comprising:
- step a) at least one step of grinding in an aqueous medium of at least one latex and at least one mineral material, b) optionally at least one suspension concentration stage resulting from step a), with possibly at least one a dispersant, c) optionally at least one step of drying the suspension resulting from step a) or b),
- step a) 1) in that it is introduced into the aqueous medium before and / or during step a), 2) and in that it comprises:
- Ethyl acrylate is an unsaturated amide and very preferably acrylamide.
- Concentration is understood to mean a step intended to increase the dry matter content of the suspension, such as, for example, filtration or centrifugation or any other mechanical means of reconcentration.
- water-soluble copolymer comprises, expressed as a percentage by weight of each of the monomers (the total of these percentages being equal to 100%):
- This use is also characterized in that the monomer 2.1) is chosen from acrylic acid, methacrylic acid and mixtures thereof.
- the monomer 2.2) is a monomer of formula (I): or m, n, p are integers less than 150 and at least one of them is greater than 0, q is an integer greater than 0, which preferentially satisfy ⁇ (m + n + p) q ⁇
- R is a radical having a polymerizable unsaturated functional group
- R 1 and R 2 are identical or different and represent hydrogen atoms or alkyl groups
- R 1 represents a hydrophobic chain alkyl, alkylaryl, arylalkyl, aryl having
- this use is also characterized in that R 'represents a branched alkyl chain having from 10 to 24 carbon atoms and is the result of a condensation of linear alcohols according to a Guerbet reaction, and is preferentially 2-hexyl-1-decanyl, 2-octyl-1-dodecanyl and mixtures thereof.
- this use is also characterized in that R 'represents a polystyryl phenol, and preferentially a distyryl phenol, a tristyryl phenol, and mixtures thereof.
- R is chosen from vinyl functional groups, acrylic, methacrylic, maleic, unsaturated urethane esters and preferably from acrylurethane, methacrylurethane, ⁇ - ⁇ -dimethylisopropenyl-benzylurethane, polyurethane, allyl ethers. or vinyl substituted or unsubstituted, ethylenically unsaturated amides and imides, and is preferably the methacrylic ester function.
- said water-soluble copolymer has a molar neutralization level of its acid functional groups of between 0 and 50%, preferably 0 and 35%, very preferably 0 and 20%.
- water-soluble copolymer when partially acidic, is partially neutralized by one or more neutralization agents having a monovalent function or a polyvalent function, preferably chosen from sodium hydroxides, of potassium, lithium and their mixtures.
- neutralization agents having a monovalent function or a polyvalent function, preferably chosen from sodium hydroxides, of potassium, lithium and their mixtures.
- This use is also characterized in that the mineral material used is chosen from natural or synthetic calcium carbonate and their mixtures and in that it is preferably a natural calcium carbonate.
- binder used is chosen from natural binders and preferably from starch, casein, proteins, cellulose, CMC (carboxymethyl cellulose), EHEC (hydroxyethyl cellulose) or among synthetic binders and preferably acrylic, styrenic, styrene-acrylic, or mixtures thereof.
- the measurement of the TOC is carried out on each aqueous suspension of hybrid particles, after grinding, and after filtration: the filtration water is recovered on which the measurement of TOC is carried out.
- SHIMADZU TM under the name Total Organic Carbon Analyzer TOC-VCSH, supplemented by the ASI-V Autosampler and TOC-Control V software (SHIMADZU TM).
- a standard solution containing 1000 ppm of Total Carbon is prepared in a vial of
- a standard solution containing 1000 ppm of Inorganic Carbon is prepared in a 1 L flask, where 4.41 grams of sodium carbonate (previously dried in an oven at 280 ° C and cooled in a desiccator) is weighed and 3.5 grams of sodium hydrogencarbonate, and where complete to the mark.
- Calibration lines from 0 to 100 ppm for Total Carbon are performed from the TC-100-23082006.cal procedure, and from 0 to 50 ppm for Inorganic Carbon from the IC50-23082006.cal procedure.
- the Total Organic Carbon content is obtained from the TOC-280820006.met procedure.
- concentrations of the polymers are given in% by dry weight of polymer relative to the dry weight of mineral matter.
- all of the polymers of the invention are partially neutralized so that 10 mol% of their carboxylic sites are neutralized by the sodium ion.
- soda is added at the time of the dispersion step, so as to regulate the pH to a value between 8.5 and 10.
- This example relates to the manufacture of an aqueous suspension of hybrid particles of calcium carbonate and a binder, through a grinding step involving a coupling agent and a concentration step involving a dispersing agent.
- the granulometric characteristics of the suspension obtained are determined, and in particular the percentages by weight of particles having an average diameter of less than 1 ⁇ m and 2 ⁇ m, respectively denoted% ⁇ 1 ⁇ m and% ⁇ 2 ⁇ m (from one apparatus of the Sedigraph TM 5100 type sold by the company MICROMERITICS TM).
- Each suspension is then filtered on a B ⁇ chner TM filter press: a filter cake is obtained. This is then dispersed so as to obtain a solids content equal to 50% of its total weight. This step takes place in the presence of a dispersing agent.
- coupling agent # 1 0.5% by dry weight of Polygen TM WE 4 referred to as coupling agent # 1, referred to as AGI, and as dispersant:
- the TOC value is equal to 1217 ppm, which is very high: this indicates a weak self-binding character at the level of the hybrid particles manufactured and therefore unsatisfactory for those skilled in the art; from then on, we did not try to disperse or reconcentrate the environment.
- the coupling agent 0.5% by dry weight of a homopolymer of acrylic acid with a molecular weight of 11 000 g / mol, referred to as coupling agent No. 3 and denoted AG3,
- the value of TOC is here extremely high (greater than 12,000 ppm): it is likely that we have not managed to make self-binding particles. So we did not try to disperse or re-concentrate the medium.
- ADl copolymer 0.5% by dry weight of the ADl copolymer (which will also be noted as AG4).
- TOC is equal to 688 ppm, which remained very high: this reflects a weak self-binding character at the hybrid particles manufactured and therefore unsatisfactory to the skilled person; from then on, we did not try to disperse or reconcentrate the environment.
- Test No. 5 This test is outside the invention and uses:
- a coupling agent 0.5% by dry weight of a copolymer consisting of (by weight) 14% of acrylic acid, 5% of methacrylic acid and 81% of methoxy polyethylene glycol methacrylate with a molecular weight of 2 000 g / mol, called coupling agent No. 5 and denoted AG5, and as dispersant 0.6% by dry weight of the copolymer ADl, and 0.1% by dry weight of the copolymer AD2.
- the TOC value remains high (451 ppm): the self-binding nature of the manufactured hybrid particles is weak; this being, it is more important than for the tests n ° 2, 3 and 4: one thus sought to redisperse the medium.
- the value of TOC is equal to 300 which remains high, but less than for previous tests; in this particular case, we therefore sought to find the medium.
- This example relates to the manufacture of an aqueous suspension of hybrid particles of calcium carbonate and a binder, through a grinding step involving a coupling agent and a concentration step involving a dispersing agent.
- This example relates to the manufacture of an aqueous suspension of hybrid particles of calcium carbonate and a binder, through a single grinding step involving a coupling agent, without subsequent concentration phase.
- Example 2 The procedure is carried out according to the method described in Example 1, with the difference that the grinding is carried out so as to obtain a final solids content of 70%.
- the suspension is filtered after grinding and the TOC is measured on the filtration water.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0950247A FR2941235B1 (fr) | 2009-01-16 | 2009-01-16 | Utilisation de polymeres acryliques peigne avec des groupes hydrophobes comme agents de couplage dans un procede de broyage de matieres minerales avec des liants. |
PCT/IB2010/000034 WO2010082107A1 (fr) | 2009-01-16 | 2010-01-06 | Utilisation de polymeres acryliques peigne avec des groupes hydrophobes comme agents de couplage dans un procede de broyage de matieres minerales avec des liants |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2387601A1 true EP2387601A1 (fr) | 2011-11-23 |
Family
ID=41257104
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10701720A Withdrawn EP2387601A1 (fr) | 2009-01-16 | 2010-01-06 | Utilisation de polymeres acryliques peigne avec des groupes hydrophobes comme agents de couplage dans un procede de broyage de matieres minerales avec des liants |
Country Status (5)
Country | Link |
---|---|
US (1) | US8191807B2 (fr) |
EP (1) | EP2387601A1 (fr) |
CN (1) | CN102282228A (fr) |
FR (1) | FR2941235B1 (fr) |
WO (1) | WO2010082107A1 (fr) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2456369T3 (es) | 2011-08-31 | 2014-04-22 | Omya International Ag | Híbrido de pigmentos autoaglutinantes |
US9074067B2 (en) | 2011-12-22 | 2015-07-07 | Rohm And Haas Company | Calcium carbonate slurries |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2842814B1 (fr) * | 2002-07-26 | 2004-10-22 | Coatex Sas | Procede de polymerisation radicalaire controlee de l'acide acrylique et de ses sels, les polymeres obtenus, et leurs applications. |
FR2846978B1 (fr) * | 2002-11-08 | 2007-05-18 | Coatex Sas | Utilisation d'un copolymere disposant d'au moins une fonction greffee alkoxy ou hydroxy polyalkylene glycol, comme agent ameliorant l'activation de l'azurage optique et produits obtenus |
FR2873127B1 (fr) * | 2004-07-13 | 2008-08-29 | Omya Development Ag | Procede de fabrication de particules pigmentaires autoliantes, seches ou en suspension ou dispersion aqueuses, contenant des matieres inorganiques et des liants |
FR2873047B1 (fr) * | 2004-07-13 | 2007-10-05 | Coatex Soc Par Actions Simplif | Procede de broyage de matieres minerales en presence de liants, suspensions aqueuses obtenues et leurs utilisations |
DE102005025374A1 (de) | 2005-05-31 | 2006-12-07 | Basf Ag | Polymer-Pigment-Hybride für die Papierherstellung |
FR2913420B1 (fr) * | 2007-03-05 | 2009-05-01 | Coatex Soc Par Actions Simplif | Utilisation dans une composition de liant hydraulique,d'un carbonate de calcium broye a sec avec un copolymere de l'acide (meth) acrylique et une fonction alcoxy ou hydroxy polyalkyleneglycol. |
GB0707457D0 (en) * | 2007-04-17 | 2007-05-23 | Imerys Minerals Ltd | Grinding method |
DE602007014018D1 (de) | 2007-05-11 | 2011-06-01 | Omya Development Ag | Mahlverfahren für mineralische Materialien und Bindemittel in einem wässrigen Medium unter Einsatz einer inversen Emulsion aus einem Acrylamidpolymer mit einem Acrylmonomer |
-
2009
- 2009-01-16 FR FR0950247A patent/FR2941235B1/fr not_active Expired - Fee Related
-
2010
- 2010-01-06 WO PCT/IB2010/000034 patent/WO2010082107A1/fr active Application Filing
- 2010-01-06 EP EP10701720A patent/EP2387601A1/fr not_active Withdrawn
- 2010-01-06 CN CN2010800046166A patent/CN102282228A/zh active Pending
- 2010-01-19 US US12/689,631 patent/US8191807B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
See references of WO2010082107A1 * |
Also Published As
Publication number | Publication date |
---|---|
FR2941235A1 (fr) | 2010-07-23 |
US20100181395A1 (en) | 2010-07-22 |
CN102282228A (zh) | 2011-12-14 |
US8191807B2 (en) | 2012-06-05 |
FR2941235B1 (fr) | 2011-01-14 |
WO2010082107A1 (fr) | 2010-07-22 |
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