WO2020120169A1 - Dispersions aqueuses et poudres de dispersion à base de microsilice - Google Patents

Dispersions aqueuses et poudres de dispersion à base de microsilice Download PDF

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Publication number
WO2020120169A1
WO2020120169A1 PCT/EP2019/083036 EP2019083036W WO2020120169A1 WO 2020120169 A1 WO2020120169 A1 WO 2020120169A1 EP 2019083036 W EP2019083036 W EP 2019083036W WO 2020120169 A1 WO2020120169 A1 WO 2020120169A1
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WO
WIPO (PCT)
Prior art keywords
microsilica
dispersion
aqueous dispersions
mol
particles according
Prior art date
Application number
PCT/EP2019/083036
Other languages
German (de)
English (en)
Inventor
Abdulmajid Hashemzadeh
Konrad Mautner
Original Assignee
Wacker Chemie Ag
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 Wacker Chemie Ag filed Critical Wacker Chemie Ag
Publication of WO2020120169A1 publication Critical patent/WO2020120169A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/146—After-treatment of sols
    • C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0042—Powdery mixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0045—Polymers chosen for their physico-chemical characteristics
    • C04B2103/0057—Polymers chosen for their physico-chemical characteristics added as redispersable powders
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0045—Polymers chosen for their physico-chemical characteristics
    • C04B2103/0066—Film forming polymers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
    • C04B2103/0082—Segregation-preventing agents; Sedimentation-preventing agents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00482—Coating or impregnation materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/10—Compositions or ingredients thereof characterised by the absence or the very low content of a specific material
    • C04B2111/1037—Cement free compositions, e.g. hydraulically hardening mixtures based on waste materials, not containing cement as such
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/72—Repairing or restoring existing buildings or building materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • Aqueous dispersions and dispersible polymer powders from microsilica are Aqueous dispersions and dispersible polymer powders from microsilica
  • the invention relates to aqueous dispersions and dispersion powder of microsilica, processes for their preparation and their use.
  • Microsilica (silica fume, silica dust) is an extremely fine-grained, mineral substance that is created, for example, as filter dust in the manufacture of silicon.
  • the starting material for this is quartz, which together with coal is reduced to metallic silicon in electric arc furnaces.
  • the resulting silicon monoxide reacts with the oxygen contained in the furnace air and S1O 2 is again formed as a by-product, which is present in the finest pearls (silica fume) and is called microsilica.
  • Microsilica is an artificial pozzolana and is used as an additive in the construction industry. It reacts with calcium hydroxide, the hydration product of cement and water, to form calcium silicate hydrate and leads to an improvement in the mechanical properties, for example the concrete pressure resistance, of the hardened cementitious masses. In addition, an improvement in the tightness and chemical resistance, for example against the penetration of chlorides, of building materials can be achieved.
  • Microsilica is available in powder form or in aqueous dispersion. For large-scale commercial use in the construction industry, it is necessary to offer microsilica in a safe, easy-to-use form that can be transported using pumps, for example. These requirements are best met by providing microsilica in the form of an aqueous dispersion. To the shipping and storage costs to minimize, it is desirable to use microsilica dispersions with a high solids concentration, that is to say with a proportion of at least 30% by weight of microsilica particles.
  • microsilica dispersions with such high solids concentrations tend to sediment and gel. Since the use in the construction industry often results in transport and storage times of up to several weeks, the prevention of sedimentation and gelation is of particular importance.
  • microsilica dispersions with a combination of complexing agent, for example EDTA, and anionic dispersing agent, for example naphthalene sulfonate-formaldehyde condensation polymer, and setting a pH of 5.0 to 8.5 to improve.
  • complexing agent for example EDTA
  • anionic dispersing agent for example naphthalene sulfonate-formaldehyde condensation polymer
  • setting a pH of 5.0 to 8.5 to improve.
  • EDTA is added for stabilization and a pH of 3 to 6 is set.
  • US 4,888,058 tripolyphosphate and / or citric acid and their salts are used to stabilize the microsilica dispersions.
  • US 2005/0167105 A1 microsilica particles are used as granules, which are bound with biodegradable polymers, for example cellulose.
  • WO 2018/052307 A1 describes aqueous microsilica dispersions which are stabilized by adjusting the pH to a range from 4 to 7 and adding polylactic acid. The problem with all of these processes is that the additives used delay the hydraulic bonding in cementitious materials or pollute the environment.
  • the invention relates to aqueous dispersions and dispersion powders of microsilica particles, characterized in that they are stabilized with vinyl alcohol copolymer.
  • Microsilica is a fine-grained silicon dioxide that fulfills the requirements and conformation criteria according to DIN EN 13263-1.
  • the microsilica particles preferably have an average primary particle particle size d-PP of 45 mth, determined by means of statistical laser diffraction analysis.
  • the microsilica products mentioned are commercially available, for example from Elkem ASA.
  • Vinyl alcohol copolymers with are suitable for stabilization
  • Most preferred as monomers c) are vinyl sulfonic acid, 2-acrylamido-2-methylpropanesulfonic acid, and their salts.
  • Suitable monomers d) are vinyl propionate, vinyl butyrate, vinyl 2-ethylhexanoate, vinyl laurate, 1-methyl vinyl acetate and vinyl esters of o-branched monocarboxylic acids with 5 to 13 carbon atoms, for example vinyl pivalate, VeoVa9 R , VeoVal0 R or Ve- oVall R (trade name of Hexion).
  • the vinyl esters of a-branched monocarboxylic acids with 9 to 10 carbon atoms (VeoVa9 R and VeoVal0 R ) are preferred.
  • the vinyl alcohol polymers can be prepared in a known manner by means of free-radical polymerization of vinyl acetate, if appropriate using the comonomers mentioned under c) and d) and then hydrolysing the polymers obtained in this way.
  • Suitable polyvinyl alcohols and sulfonated polyvinyl alcohols are also commercially available.
  • the aqueous dispersions of microsilica particles contain 20 to 60% by weight, preferably 30 to 50% by weight, of microsilica, in each case based on the sum of the parts by weight of microsilica and water.
  • the amount of vinyl alcohol copolymer in the aqueous microsilica dispersion or in the microsilica dispersion powder is 1 to 20 wt .-%, preferably 3 to 10 wt .-% vinyl alcohol copolymer, each based on the proportion by weight of microsilica ver in the dispersion or in the dispersion powder.
  • the procedure is preferably such that the vinyl alcohol copolymer is initially dissolved in water and the powdery microsilica particles are added to this solution and dispersed.
  • the microsilica particles can be packaged, for example in sacks, or stored in bulk, for example in silos or large containers.
  • the microsilica particles can be added via sack dumpers, dosing loos with and without weighing or by direct conveyance from storage silos or large containers using suitable conveyor systems such as compressed air diaphragm pumps.
  • suitable conveyor systems such as compressed air diaphragm pumps.
  • the microsilica particles are incorporated by shaking, for example using a tumble mixer or a high-speed mixer, or by stirring, for example using a bar stirrer or dissolver.
  • the microsilica particles can be dispersed subsequently or in parallel with the addition of the microsilica particles.
  • Parallel dispersion means that when the microsilica particles begin to be metered into the aqueous phase, the dispersion process begins.
  • High-speed stirrers, high-speed dissolvers, for example with circulation speeds of 1 to 50 m / s, high-speed rotor-stator systems, sonolators, shear gaps, nozzles or ball mills are preferably suitable for this.
  • the use of ultrasound in the range from 5 Hz to 500 kHz is suitable for dispersing the microsilica particles.
  • the dispersion can be carried out by combining various methods, e.g. Predispersion using a dissolver or inductor followed by fine dispersion using ultrasound treatment.
  • the production can be carried out in batch and continuous processes. Continuous processes are preferred.
  • the aqueous microsilica dispersions are adjusted to a pH of 6 to 8.
  • the aqueous dispersion of the microsilica particles can be dried, for example, by means of fluidized-bed drying, freeze-drying or spray drying.
  • the microsilica dispersions are preferably spray-dried.
  • aqueous dispersions or water-dispersible dispersion powders of microsilica particles are suitable for use in cementitious or non-cemented building materials, in pasty form or as dry mortar. Examples of building materials are plasters, mortar, screeds and concrete.
  • the aqueous dispersions or dispersion powders of microsilica particles are also suitable for use in adhesives, sealants, fillers and paints.
  • a monomer mixture 1 with 999 g VeoVa R 10 and 18661 g vinyl acetate was metered in with a metering time of 180 minutes.
  • a monomer solution 2 from 1319 g of a 25% aqueous solution of vinyl sulfonate was metered in with a metering time of 195 minutes.
  • the reactor was locked, the pressure in the reactor was increased to 0.2 bar and post-polymerized at 100 ° C. for one hour.
  • the polymer solution was then cooled to 30 ° C. and diluted with methanol to a 31% by weight solution.
  • the polymer solution was overlaid without stirring with 38440 g of methanol and then a mixture of 775 g of methanol and 657 g of 46% sodium hydroxide solution was added and stirred. After two hours the solution was neutralized with 342 g acetic acid (99.8%). Then methanol and the by-products were removed by steam stripping. After stripping, the vinyl alcohol copolymer was taken up in water and diluted to a 20% by weight solution.
  • Polyvinyl alcohol 2 (PVOH 2): A 20% aqueous solution of a vinyl alcohol copolymer with 88 mol% vinyl alcohol and 12 mol% vinyl acetate monomer units was used as PVOH 2.
  • microsilica dispersions produced were stored closed at room temperature. After 24 hours, it was examined whether a phase separation (sedimentation) had taken place.
  • microsilica dispersions were dried at room temperature. After drying, the microsilica dispersion powder obtained was ground and sieved (mesh size of 1 mm).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne des dispersions aqueuses et des poudres de dispersion à base de particules de microsilice, caractérisées en ce qu'elles sont stabilisées avec un copolymère d'alcool vinylique.
PCT/EP2019/083036 2018-12-11 2019-11-29 Dispersions aqueuses et poudres de dispersion à base de microsilice WO2020120169A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102018221446.8A DE102018221446A1 (de) 2018-12-11 2018-12-11 Wässrige Dispersionen und Dispersionspulver von Mikrosilika
DE102018221446.8 2018-12-11

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Publication Number Publication Date
WO2020120169A1 true WO2020120169A1 (fr) 2020-06-18

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PCT/EP2019/083036 WO2020120169A1 (fr) 2018-12-11 2019-11-29 Dispersions aqueuses et poudres de dispersion à base de microsilice

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DE (1) DE102018221446A1 (fr)
WO (1) WO2020120169A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4321243A (en) 1980-08-05 1982-03-23 Cornwell Charles E Method of producing stabilized aqueous dispersions of silica fume
EP0246181A1 (fr) 1986-05-13 1987-11-19 W.R. Grace & Co. Boues de microsilice et procédé de préparation
US4888058A (en) 1986-09-29 1989-12-19 W. R. Grace & Co.-Conn. Silica fume slurry
US6653372B1 (en) * 1996-06-12 2003-11-25 Basf Aktiengesellschaft Preparation of addition-polymer powder
US20040097645A1 (en) * 2002-11-14 2004-05-20 Wacker Polymer Systems Gmbh & Co. Kg Protective-colloid-stabilized polymers in the form of their aqueous dispersions or of their water-redispersible powders
US20050167105A1 (en) 2004-01-30 2005-08-04 Roddy Craig W. Contained micro-particles for use in well bore operations
US20070213430A1 (en) * 2003-10-09 2007-09-13 Werner Bauer Polymeric compositions containing modified polyvinyl alcohols
US20140243457A1 (en) * 2011-10-05 2014-08-28 Wacker Chemie Ag Dry building material formulations containing polymer powders
WO2018052307A1 (fr) 2016-09-13 2018-03-22 Elkem As Suspension de microsilice et procédé de production d'une telle suspension

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4321243A (en) 1980-08-05 1982-03-23 Cornwell Charles E Method of producing stabilized aqueous dispersions of silica fume
EP0246181A1 (fr) 1986-05-13 1987-11-19 W.R. Grace & Co. Boues de microsilice et procédé de préparation
US4888058A (en) 1986-09-29 1989-12-19 W. R. Grace & Co.-Conn. Silica fume slurry
US6653372B1 (en) * 1996-06-12 2003-11-25 Basf Aktiengesellschaft Preparation of addition-polymer powder
US20040097645A1 (en) * 2002-11-14 2004-05-20 Wacker Polymer Systems Gmbh & Co. Kg Protective-colloid-stabilized polymers in the form of their aqueous dispersions or of their water-redispersible powders
US20070213430A1 (en) * 2003-10-09 2007-09-13 Werner Bauer Polymeric compositions containing modified polyvinyl alcohols
US20050167105A1 (en) 2004-01-30 2005-08-04 Roddy Craig W. Contained micro-particles for use in well bore operations
US20140243457A1 (en) * 2011-10-05 2014-08-28 Wacker Chemie Ag Dry building material formulations containing polymer powders
WO2018052307A1 (fr) 2016-09-13 2018-03-22 Elkem As Suspension de microsilice et procédé de production d'une telle suspension

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