US20070068088A1 - Use of polymeric microparticles in building material mixtures - Google Patents

Use of polymeric microparticles in building material mixtures Download PDF

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Publication number
US20070068088A1
US20070068088A1 US11/247,962 US24796205A US2007068088A1 US 20070068088 A1 US20070068088 A1 US 20070068088A1 US 24796205 A US24796205 A US 24796205A US 2007068088 A1 US2007068088 A1 US 2007068088A1
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United States
Prior art keywords
microparticles
concrete
water
volume
air
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Abandoned
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US11/247,962
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English (en)
Inventor
Lars Einfeldt
Gerhard Albrecht
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Roehm GmbH Darmstadt
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Individual
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Assigned to CONSTRUCTION RESEARCH & TECHNOLOGY GMBH reassignment CONSTRUCTION RESEARCH & TECHNOLOGY GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ALBRECHT, GERHARD, EINFELDT, LARS
Assigned to ROHM GMBH reassignment ROHM GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CONSTRUCTION RESEARCH & TECHNOLOGY GMBH
Publication of US20070068088A1 publication Critical patent/US20070068088A1/en
Priority to US12/290,880 priority Critical patent/US8177904B2/en
Assigned to EVONIK ROHM GMBH reassignment EVONIK ROHM GMBH CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: ROHM GMBH
Abandoned legal-status Critical Current

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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
    • 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
    • C04B20/0016—Granular materials, e.g. microballoons
    • C04B20/002—Hollow or porous granular materials
    • C04B20/0036—Microsized or nanosized
    • 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
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2641—Polyacrylates; Polymethacrylates
    • 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
    • C04B2103/0049—Water-swellable 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
    • C04B2103/0045—Polymers chosen for their physico-chemical characteristics
    • C04B2103/0058—Core-shell 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
    • 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
    • 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

Definitions

  • the present invention relates to the use of polymeric microparticles in hydraulically setting building material mixtures for improving the frost resistance thereof or the resistance thereof to the freezing and thawing cycle.
  • Capillary pores (radius: 2 ⁇ m-2 mm) or gel pores (radius: 2-50 nm) pass through the texture of a cement-bound concrete. Pore water contained therein differs in its state depending on the pore diameter.
  • a precondition for improved resistance of concrete to the freezing and thawing cycle is that the distance of each point in the hardened cement base from the next artificial air pore does not exceed a certain value. This distance is also referred to as the “Powers spacing factor” [T. C. Powers, 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 “Powers spacing factor” of 500 ⁇ m leads to damage to the concrete in the freezing and thawing cycle. In order to achieve this with a limited air pores 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 systems characterization, “ Material Science of Concrete ” VI (2001) 129-214].
  • an artificial air pore system depends decisively on the composition and the particle shape of the additives, the type and amount of the cement, the concrete consistency, the mixer used, the mixing time, the temperature, but also the type and amount of the air-entraining agent. Taking into account appropriate production rules, it is possible to control the influences thereof, but a multiplicity of undesired adverse effects may occur, which in the end means that the desired air content in the concrete may be exceeded or not reached and hence adversely affects the strength or the frost resistance of the concrete.
  • sodium oleate the sodium salt of abietic acid or vinsol resin, an extract from pine roots—reacts with the calcium hydroxide of the pore solution in the cement paste and is precipitated as insoluble calcium salt.
  • These hydrophobic salts reduce the surface tension of the water and collect at the interface between cement particles, air and water. They stabilize the microbubbles and are therefore present on the surfaces of these air pores in the hardened concrete.
  • the other type e.g. sodium laurylsulfate (SDS) or sodium dodecylphenylsulfonate—forms soluble calcium salts with calcium hydroxide, which calcium salts, however, exhibit abnormal solution behavior.
  • these surfactants have a very low solubility; above this temperature, they are very readily soluble. By preferentially collecting at the air/water boundary, they also reduce the surface tension and thus stabilize the microbubbles and are preferably present at the surfaces of these air pores in the hardened concrete.
  • microparticles described therein are distinguished in particular by the fact that they have a cavity which is smaller than 200 ⁇ m (diameter), and this hollow core consists of air (or a gaseous substance). This also includes porous microparticles of the 100 ⁇ m scale, which may have a multiplicity of relatively small cavities and/or pores.
  • This object was achieved, according to the invention, by using microparticles whose cavity is filled with from 1 to 100% by volume of water.
  • polymeric microparticles whose cavity is filled with from 1 to 100% by volume, in particular from 10 to 100% by volume, of water are used.
  • the microparticles used consist of polymer particles which contain a polymer core (A) based on an unsaturated carboxylic acid (derivative) monomer and a polymer shell (B) based on a nonionic, ethylenically unsaturated monomer, the core/shell polymer particles having been swollen with the aid of a base.
  • the unsaturated carboxylic acid (derivative) monomers preferably consist of a compound selected from the group consisting of acrylic acid, methacrylic acid, maleic acid, maleic anhydride, fumaric acid, itaconic acid and crotonic acid.
  • styrene, butadiene, vinyltoluene, ethylene, vinyl acetate, vinyl chloride, vinylidene chloride, acrylonitrile, acrylamide, methacrylamide, C 1 -C 12 -alkyl esters of acrylic or methacrylic acid are used as nonionic, ethylenically unsaturated monomers which form the polymer shell (B).
  • microparticles used according to the invention have a preferred diameter of from 0.1 to 20 ⁇ m.
  • the polymer content of the microparticles used may be from 2 to 98% by weight, depending on the diameter and the water content.
  • microparticles for example of the type ROPAQUE®
  • aqueous dispersion which must contain a certain proportion of dispersant having a surfactant structure in order to suppress agglomeration of the microparticles.
  • dispersions of these microparticles which comprise no surface-active surfactants (which may have a disturbing effect in the concrete).
  • the microparticles are dispersed in aqueous solutions which comprise a rheological standardizing agent.
  • Such thickening agents which have a pseudoplastic viscosity, are generally of a polysaccharide nature [D. B. Braun & M. R.
  • the surfactants dissolved in the aqueous dispersion can be separated off by first coagulating the microparticles, for example with calcium chloride (CaCl 2 ) and then washing them with water. Finally, redispersion in any desired thickening dispersant is possible.
  • CaCl 2 calcium chloride
  • the water-filled, polymeric microparticles are used in the form of an aqueous dispersion (with or without surfactants).
  • the microparticles are coagulated and are isolated from the aqueous dispersion by customary methods (e.g. filtration, centrifuging, sedimentation and decanting) and the particles are then dried, with the result that the water-containing core can certainly be retained.
  • washing of the coagulated material with readily volatile liquids may be helpful.
  • alcohols such as MeOH or EtOH, have proven useful.
  • the water-filled microparticles are added to the building material mixture in a preferred amount of from 0.01 to 5% by volume, in particular from 0.1 to 0.5% by volume.
  • the building material mixture for example in the form of concrete or mortar, may contain the customary hydraulically setting binders, such as, for example, cement, lime, gypsum or anhydrite.
  • a substantial advantage of the use of the water-filled microparticles is that only an extremely small amount of air is introduced into the concrete.
  • Substantially improved compressive strengths of the concrete can be achieved as a result. These are about 25-50% above the compressive strengths of concrete which was obtained with conventional air entrainment.
  • W/C value water/cement value
  • low W/C values in turn may substantially limit the processibility of the concrete.
  • the result of higher compressive strengths may be that the cement content in the concrete which is required for strength development can be reduced and hence the price per m 3 of concrete is significantly reduced.
  • a different water content in the core of the individual ROPAQUE® type was produced by differentiated drying. It is dependent on the drying temperature, the drying time and the low pressure (vacuum) used.
  • the water content in the interior of the microparticles can be determined by Karl Fischer titration if the externally dried (poly)styrene shell was previously dissolved in a suitable solvent (e.g. anhydrous acetone). If a coagulated ROPAQUE® dispersion is washed first with water and then with methanol, the enclosed proportion of water (100% by volume) of the ROPAQUE® microparticles can be virtually completely determined with the aid of the Karl Fischer titration by simple and rapid air drying at room temperature and atmospheric pressure.
  • a suitable solvent e.g. anhydrous acetone
  • the water content determined does not agree exactly with the actual water content in the microparticles, since there is always a time gap between determination of the water content and use of the concrete, during which water (or water vapor) can diffuse out of the cavity through the shell of the microparticles. Even in the case of testing close to the time of use, the stated water content can therefore only be a guide value.
  • a commercial dispersion sample comprising microparticles of the type ROPAQUE®, corresponding to ASTM C 666 (procedure A), was added to the concrete and the latter was exposed to 180 freezing-and-thawing cycles in a freezing-thawing chamber.
  • the plastic air content of the concrete was determined and the compressive strength of the concretes were determined after 7 and 28 days.
  • the values determined for the resistance to the freezing and thawing cycle of the concrete should not differ by more than 10% from the reference (classical air-entraining agent). In other words, all values determined >90 (reference: 99) means sufficient protection of the concrete from frost damage.
  • microparticles “surfactant-free” according to example 2, of a commercial ROPAQUE® type were dispersed in a rheological standardizing agent (0.4% strength by weight diutan solution) in order to suppress the agglomeration of the dried microparticles in the water or cement paste.
  • these microparticles in the form of a 20% strength by weight dispersion in a 0.4% strength by weight diutan solution, were added to the mixer and subjected again to 180 freezing-and-thawing cycles according to ASTM 666 C (procedure A). The following variations were implemented:
  • the freezing/thawing cycle resistance factor is based on ASTM 666 C (procedure A). (The values determined for the resistance of the concrete to the freezing and thawing cycle should not deviate by more than 10% from the reference (classical air-entraining agent). In other words, all determined values > 90 mean sufficient protection of the concrete from frost damage.)
  • the weathering factor is a qualitative measure of the optically visible frost damage and is subject to a visual rating on the scale 0 (good) to 5 (poor). (A concrete having good resistance to the freezing and thawing cycle should be given at least the rating 3.)
  • the freezing/thawing cycle resistance factor is based on ASTM 666 C (procedure A). (The values determined for the resistance of the concrete to the freezing and thawing cycle should not deviate by more than 10% from the reference (classical air-entraining agent). In other words, all determined values > 90 mean sufficient protection of the concrete from frost damage.)
  • the weathering factor is a qualitative measure of the optically visible frost damage and is subject to a visual rating on the scale 0 (good) to 5 (poor). (A concrete having good resistance to the freezing and thawing cycle should be given at least the rating 3.)
  • the values determined for the resistance of the concrete to the freezing and thawing cycle should not deviate by more than 10% from the reference (classical air-entraining agent). In other words, all determined values > 90 mean sufficient protection of the concrete from frost damage.
  • the weathering factor is a qualitative measure of the optically visible frost damage and is subject to a visual rating on the scale 0 (good) to 5 (poor). (A concrete having good resistance to the freezing and thawing cycle should be given at least the rating 3.)

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  • 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)
  • Nanotechnology (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
US11/247,962 2005-09-29 2005-10-11 Use of polymeric microparticles in building material mixtures Abandoned US20070068088A1 (en)

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US12/290,880 US8177904B2 (en) 2005-09-29 2008-11-04 Use of polymeric microparticles in building material mixtures

Applications Claiming Priority (2)

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DE102005046681.8 2005-09-29
DE102005046681A DE102005046681A1 (de) 2005-09-29 2005-09-29 Verwendung von polymeren Mikropartikeln in Baustoffmischungen

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US (2) US20070068088A1 (enExample)
EP (1) EP1928801A1 (enExample)
JP (1) JP5260293B2 (enExample)
CN (1) CN101304958A (enExample)
CA (1) CA2623881C (enExample)
DE (1) DE102005046681A1 (enExample)
WO (1) WO2007036365A1 (enExample)

Cited By (28)

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US20040116567A1 (en) * 2001-02-07 2004-06-17 Gunter Schmitt Hot sealing compound for aluminum foils applied to polypropylene and polystyrene
US20070117948A1 (en) * 2003-10-29 2007-05-24 Roehm Gmbh & Co. Kg Mixtures for producing reactive hot melt adhesives and reactive hot melt adhesives obtained on the basis thereof
US20070193156A1 (en) * 2006-02-23 2007-08-23 Roehm Gmbh & Co. Kg Additive building material mixtures containing spray-dried microparticles
US20070193159A1 (en) * 2006-02-23 2007-08-23 Roehm Gmbh & Co. Kg Additive building material mixtures containing different-sized microparticles
US20070197671A1 (en) * 2006-02-23 2007-08-23 Roehm Gbmh & Co. Kg Additive building material mixtures containing microparticles having very thin shells
US20070197691A1 (en) * 2006-02-23 2007-08-23 Roehm Gmbh & Co. Kg Additive building material mixtures containing ionic emulsifiers
US20070197690A1 (en) * 2006-02-23 2007-08-23 Roehm Gbmh & Co. Kg Additive building material mixtures containing sterically or electrostatically repulsive monomers in the microparticles' shell
US20070193478A1 (en) * 2006-02-23 2007-08-23 Roehm Gbmh & Co. Kg Additive building material mixtures containing microparticles having non-polar shells
US20070204543A1 (en) * 2006-03-01 2007-09-06 Roehm Gmbh & Co. Kg Additive building material mixtures containing ionically swollen microparticles
US20070204544A1 (en) * 2006-03-01 2007-09-06 Roehm Gmbh & Co. Kg Additive building material mixtures containing solid microparticles
US20070208109A1 (en) * 2006-03-01 2007-09-06 Roehm Gbmh & Co., Kg Additive building material mixtures containing swellable polymeric formations
US20070208107A1 (en) * 2006-03-01 2007-09-06 Roehm Gbmh & Co. Kg Additive building material mixtures containing microparticles swollen in the building material mixture
US20070259987A1 (en) * 2004-07-23 2007-11-08 Roehm Gmbh Low Water-Absorption Plastisol Polymers
US20080057205A1 (en) * 2005-06-17 2008-03-06 Roehm Gmbh Heat-Sealing Compound For Sealing Aluminium Foil And Polyethlene Terephthalate Film To Polypropylene, Polyvinyl Chloride and Polystyrene Containers
US20080237529A1 (en) * 2005-10-28 2008-10-02 Evonik Roehm Gmbh Sprayable Acoustic Compositions
US20080262176A1 (en) * 2005-09-22 2008-10-23 Evonik Roehm Gmbh Process for Preparing (Meth) Acrylate-Based Aba Triblock Copolymers
US20080292893A1 (en) * 2006-02-28 2008-11-27 Evonik Roehm Gmbh Heat-Sealing Material for Aluminum Foils and Polyethylene Terephthalate Foils Against Polypropyl, Polyvinyl Chloride, and Polystyrol Containers
US20090048401A1 (en) * 2006-02-28 2009-02-19 Evonik Roehm Gmbh Synthesis of polyester-graft-poly(meth)acrylate copolymers
US20090062508A1 (en) * 2006-04-03 2009-03-05 Evonik Roehm Gmbh Copper removal from atrp products by means of addition of sulfur compounds
US20090099271A1 (en) * 2005-09-29 2009-04-16 Lars Einfeldt Use of polymeric microparticles in building material mixtures
US20090165949A1 (en) * 2006-02-16 2009-07-02 Evonik Roehm Gmbh Method of bonding materials of construction using nanoscale, superparamagnetic poly(meth)acrylate polymers
US20090275707A1 (en) * 2006-08-09 2009-11-05 Evonik Roehm Gmbh Process for preparing halogen-free atrp products
US20090292066A1 (en) * 2006-08-18 2009-11-26 Evonik Roehm Gmbh Plastisols based on a methyl methacrylate copolymer
US20090312498A1 (en) * 2006-08-09 2009-12-17 Evonik Roehm Gmbh Process for preparing hydroxy-telechelic atrp products
US20090326163A1 (en) * 2006-08-09 2009-12-31 Evonik Roehm Gmbh Process for preparing acid-terminated atrp products
US20100041852A1 (en) * 2006-10-10 2010-02-18 Evonik Roehm Gmbh Method for producing silyl telechelic polymers
US20100062271A1 (en) * 2006-11-22 2010-03-11 Evonik Roehm Gmbh Process for producing improved binders for plastisols
US20100280182A1 (en) * 2006-07-28 2010-11-04 Evonik Roehm Gmbh Method for the production of (meth) acrylate-based aba triblock copolymers

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DE102006008970A1 (de) * 2006-02-23 2007-08-30 Röhm Gmbh Additive Baustoffmischungen mit nichtionischen Emulgatoren
DE102006008968A1 (de) * 2006-02-23 2007-08-30 Röhm Gmbh Additive Baustoffmischungen mit Mikropartikeln, deren Schalen porös und/oder hydrophil sind
US8915997B2 (en) 2013-05-16 2014-12-23 Navs, Llc Durable concrete and method for producing the same
JP6163382B2 (ja) * 2013-08-16 2017-07-12 旭化成株式会社 モルタル用ラテックス、モルタル組成物、及びモルタル硬化物
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US8177904B2 (en) 2012-05-15
EP1928801A1 (de) 2008-06-11
DE102005046681A1 (de) 2007-04-05
JP2009509900A (ja) 2009-03-12
CN101304958A (zh) 2008-11-12
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US20090099271A1 (en) 2009-04-16
CA2623881A1 (en) 2007-04-05

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