EP1986973A2 - Additive baustoffmischungen mit mikropartikeln verschiedener grösse - Google Patents

Additive baustoffmischungen mit mikropartikeln verschiedener grösse

Info

Publication number
EP1986973A2
EP1986973A2 EP07712134A EP07712134A EP1986973A2 EP 1986973 A2 EP1986973 A2 EP 1986973A2 EP 07712134 A EP07712134 A EP 07712134A EP 07712134 A EP07712134 A EP 07712134A EP 1986973 A2 EP1986973 A2 EP 1986973A2
Authority
EP
European Patent Office
Prior art keywords
microparticles
polymeric
concrete
building material
voided
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Withdrawn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
EP07712134A
Other languages
German (de)
English (en)
French (fr)
Inventor
Jan Hendrik Schattka
Holger Kautz
Gerd LÖHDEN
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.)
Roehm GmbH Darmstadt
Original Assignee
Evonik Roehm GmbH
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 Evonik Roehm GmbH filed Critical Evonik Roehm GmbH
Publication of EP1986973A2 publication Critical patent/EP1986973A2/de
Withdrawn legal-status Critical Current

Links

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
    • C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/04—Macromolecular compounds
    • C04B16/08—Macromolecular compounds porous, e.g. expanded polystyrene beads or microballoons
    • C04B16/085—Macromolecular compounds porous, e.g. expanded polystyrene beads or microballoons expanded in situ, i.e. during or after mixing the mortar, concrete or artificial stone 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
    • C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/04—Macromolecular compounds
    • C04B16/08—Macromolecular compounds porous, e.g. expanded polystyrene beads or microballoons
    • 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
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0076—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials characterised by the grain distribution
    • C04B20/008—Micro- or nanosized fillers, e.g. micronised fillers with particle size smaller than that of the hydraulic binder
    • 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
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/29—Frost-thaw resistance
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y10T428/249967—Inorganic matrix in void-containing component
    • Y10T428/249968—Of hydraulic-setting material
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/254—Polymeric or resinous material
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2998—Coated including synthetic resin or polymer

Definitions

  • the present invention relates to the use of polymeric microparticles in hydraulically setting building material mixtures to improve their Frostg. Freeze-thaw resistance.
  • the concrete has two time-dependent properties. First, it experiences a decrease in volume due to dehydration, which is called shrinkage. However, most of the water is bound as water of crystallization. Concrete does not dry, it binds, that is, the initially low-viscosity cement paste (cement and water) stiffens, solidifies and finally solidifies, depending on the timing and sequence of the chemical-mineralogical reaction of the cement with the water, the hydration. Due to the water-binding capacity of the cement, the concrete, in contrast to calcined lime, can also harden under water and remain firm. Secondly, concrete deforms under load, the so-called creep.
  • the frost-thaw cycle refers to the climatic change of temperatures around the freezing point of water.
  • the frost-thaw cycle is a damaging mechanism. These materials have a porous, capillary structure and are not waterproof. If such, water-soaked structure exposed to temperatures below 0 0 C, the water freezes in the Pores. Due to the density anomaly of the water, the ice now expands. This leads to damage to the building material. In the very fine pores due to surface effects, the freezing point is lowered. In micro pores, water only freezes below -M 0 C. Since the material itself also expands and contracts due to freeze-thaw cycles, there is an additional capillary pumping effect that further increases water absorption and thus indirectly the damage. The number of freeze-thaw cycles is therefore decisive for the damage.
  • the structure of a cement-bound concrete is traversed by capillary pores (radius: 2 ⁇ m - 2 mm) or gel pores (radius: 2 - 50 nm). Pore water contained therein differs in its state form depending on the pore diameter.
  • a prerequisite for an improved resistance of the concrete during frost and thaw changes is that the distance of each point in the cement stone from the next artificial air pore does not exceed a certain value. This distance is also referred to as the "distance factor” or “powers spacing factor” [TCPowers, The air requirement of frost-resistant concrete, "Proceedings of the Highway Research Board” 29 (1949) 184-202]. Laboratory tests have shown that exceeding the critical "Power spacing factor" of 500 ⁇ m leads to damage to the concrete during frost and thaw cycles. In order to achieve this with a restricted air-pore content, the diameter of the artificially introduced air pores must therefore be less than 200-300 ⁇ m [K.Snyder, K. Natesaiyer & K.Hover, The stereological and Statistical properties of entrained air voids in concrete: A mathematical basis for air void system characterization) "Materials Science of Concrete” VI (2001) 129-214].
  • an artificial air pore system depends largely on the composition and grain size of the aggregates, the type and amount of cement, the concrete consistency, the mixer used, the mixing time, the temperature, but also on the type and amount of the air entraining agent. Under consideration of the appropriate manufacturing rules, their effects can indeed be mastered, however, there may be a large number of undesired impairments, which ultimately leads to the desired air content in the concrete can be exceeded or fallen below and thus adversely affected the strength or frost resistance of the concrete ,
  • These hydrophobic salts reduce the surface tension of the water and accumulate at the interface between cement grain, air and water. They stabilize the microbubbles and therefore find themselves in the hardening concrete on the surfaces of these air pores again.
  • the other type e.g. Sodium lauryl sulfate (SDS) or Natriumdodecylphenylsulfonat - on the other hand forms with calcium hydroxide soluble calcium salts, but show an abnormal solution behavior. Below a certain critical temperature these surfactants show a very low solubility, above this temperature they are very soluble. By preferentially accumulating at the air-water interface, they also reduce the surface tension, thus stabilizing the microbubbles, and are preferably found on the surfaces of these air voids in the hardened concrete.
  • SDS Sodium lauryl sulfate
  • Natriumdodecylphenylsulfonat forms with calcium hydroxide soluble calcium salts, but show an abnormal solution behavior. Below a certain critical temperature these surfactants show a very low solubility, above this temperature they are very soluble.
  • the content of fine substances in the concrete also impairs air entrainment. Also, interactions with defoaming agents can occur, which thus expel air voids, but also can introduce uncontrolled.
  • microparticles described therein have diameters of at least 10 microns (usually much larger) and have air or gas-filled cavities. This also includes porous particles which may be greater than 100 microns and may have a plurality of smaller voids and / or pores.
  • the present invention was therefore based on the object to provide a means for improving the frost or freeze-thaw resistance for hydraulically setting building material mixtures, which unfolds its full effectiveness even at relatively low dosages. Another object was to not or not significantly affect the mechanical strength of the building material by this means. Furthermore, the Abwittanssmine should be improved.
  • the object was achieved by the use of polymeric microparticles having a cavity in hydraulically setting building material mixtures, characterized in that at least two types of microparticles are used which have a different average particle diameter.
  • the mean particle size is determined, for example, by counting a statistically significant amount of particles on the basis of transmission electron micrographs.
  • microparticles used can be of the same type, and differ only in particle size. Preferred is a difference of average particle sizes of at least 20%. Particularly preferred is a difference in average particle sizes of at least 50%.
  • particles of various types may also be used.
  • core / shell particles produced by emulsion polymerization, with a swollen core together with hollow microspheres with a diameter of several micrometers can be used.
  • the latter are commercially available, for example, under the trade name Expancel (Akzo Nobel).
  • the microparticles can also be prepared in the synthesis with an at least bimodal particle size distribution.
  • At least one of the types of particles contained in the mixture has an average particle size of less than 1000 nm.
  • the smaller microparticles provide for a very low distance factor (“Powers spacing factor”) because the volume introduced by them is distributed over many particles and thus distributed very evenly in the building material matrix.
  • microparticles according to the invention can be prepared, for example, by emulsion polymerization and then preferably have a particle size of 100 to 5000 nm. Microparticles made by other means and used in combination with these microparticles may have significantly larger particle diameters. In the case of Expancel eg between 20 and 150 ⁇ m.
  • the particle size is determined, for example, by measuring and counting a statistically significant amount of particles on the basis of transmission electron micrographs.
  • the microparticles When prepared by emulsion polymerization, the microparticles are obtained in the form of an aqueous dispersion. Accordingly, the addition of the microparticles to the building material mixture preferably also takes place in this form.
  • microparticles are already known according to the prior art and are described in the publications EP 22 633 B1, EP 73 529 B1 and EP 188 325 B1. In addition, these microparticles are commercially sold under the brand name ROPAQUE® by Rohm & Haas.
  • the cavities of the microparticles are water-filled. Without limiting the invention to the effect, it is assumed that the water loses - at least partially - the particles when the building material mixture hardens, according to which gas-filled or air-filled hollow spheres are present.
  • This process takes place e.g. also in the use of such microparticles in paints instead.
  • the microparticles used consist of polymer particles which have a core (A) and at least one shell (B), the core / shell polymer particles having been swollen with the aid of a base.
  • the core (A) of the particle contains one or more ethylenically unsaturated carboxylic acid (derivative) monomers which allow swelling of the core; these monomers are preferably selected from the group of acrylic acid, methacrylic acid, maleic acid, maleic anhydride, fumaric acid, itaconic acid and crotonic acid and mixtures thereof. Acrylic acid and methacrylic acid are particularly preferred.
  • the shell (B) predominantly of nonionic, ethylenically unsaturated monomers.
  • Preferred such monomers are styrene, butadiene, vinyltoluene, ethylene, vinyl acetate, vinyl chloride, vinylidene chloride, acrylonitrile, acrylamide, methacrylamide, C1-C12-alkyl esters of (meth) acrylic acid or mixtures thereof.
  • core-shell particles which are mono- or multi-shelled, or whose shells have a gradient.
  • the polymer content of the microparticles used may vary depending on e.g. from the diameter, the core / shell ratio and the efficiency of swelling - are 2 to 98% by volume.
  • the water-filled, polymeric microparticles are used according to the invention preferably in the form of an aqueous dispersion
  • the microparticles for example - known to the expert Methods - coagulated and isolated from the aqueous dispersion by conventional methods (eg filtration, centrifugation, sedimentation and decanting). The material obtained can be washed to bring about a further lowering of the surfactant content and is then dried.
  • the water-filled microparticles are added to the building material mixture in a preferred amount of 0.01 to 5% by volume, in particular 0.1 to 0.5% by volume.
  • the building material mixture - for example in the form of concrete or mortar - can here the usual hydraulically setting binder such.
  • cement lime, gypsum or anhydrite.
  • the air introduced into the building material mixture can be kept extremely low.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
EP07712134A 2006-02-23 2007-01-30 Additive baustoffmischungen mit mikropartikeln verschiedener grösse Withdrawn EP1986973A2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200610008965 DE102006008965A1 (de) 2006-02-23 2006-02-23 Additive Baustoffmischungen mit Mikropartikeln verschiedener Größe
PCT/EP2007/050911 WO2007096238A2 (de) 2006-02-23 2007-01-30 Additive baustoffmischungen mit mikropartikeln verschiedener grösse

Publications (1)

Publication Number Publication Date
EP1986973A2 true EP1986973A2 (de) 2008-11-05

Family

ID=38319874

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07712134A Withdrawn EP1986973A2 (de) 2006-02-23 2007-01-30 Additive baustoffmischungen mit mikropartikeln verschiedener grösse

Country Status (10)

Country Link
US (1) US8039521B2 (enExample)
EP (1) EP1986973A2 (enExample)
JP (1) JP2009527451A (enExample)
KR (1) KR20080112203A (enExample)
CN (1) CN101024558A (enExample)
BR (1) BRPI0708220A2 (enExample)
CA (1) CA2643459A1 (enExample)
DE (1) DE102006008965A1 (enExample)
RU (1) RU2008137541A (enExample)
WO (1) WO2007096238A2 (enExample)

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KR20080112203A (ko) 2008-12-24
CA2643459A1 (en) 2007-08-30
JP2009527451A (ja) 2009-07-30
BRPI0708220A2 (pt) 2011-05-17
WO2007096238A2 (de) 2007-08-30
US20070193159A1 (en) 2007-08-23
CN101024558A (zh) 2007-08-29
RU2008137541A (ru) 2010-03-27
DE102006008965A1 (de) 2007-08-30
US8039521B2 (en) 2011-10-18
WO2007096238A3 (de) 2008-03-27

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