EP4347529A1 - Dispersionszusammensetzung mit einer dichtungsaufschlämmung auf zementbasis und einer additivmischung - Google Patents

Dispersionszusammensetzung mit einer dichtungsaufschlämmung auf zementbasis und einer additivmischung

Info

Publication number
EP4347529A1
EP4347529A1 EP22735306.7A EP22735306A EP4347529A1 EP 4347529 A1 EP4347529 A1 EP 4347529A1 EP 22735306 A EP22735306 A EP 22735306A EP 4347529 A1 EP4347529 A1 EP 4347529A1
Authority
EP
European Patent Office
Prior art keywords
dispersion
polymer
cement
alkyl
carbonate
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.)
Pending
Application number
EP22735306.7A
Other languages
English (en)
French (fr)
Inventor
Christian Schmidtke
Joachim Dengler
Florian DESCHNER
Harald Grassl
Klaus Seip
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of EP4347529A1 publication Critical patent/EP4347529A1/de
Pending 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
    • 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
    • C04B28/04—Portland cements
    • 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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/16—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 calcium sulfate cements containing anhydrite, e.g. Keene's cement
    • 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
    • C04B2103/0065—Polymers characterised by their glass transition temperature (Tg)
    • 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
    • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials

Definitions

  • Dispersion composition comprising a cement-based sealing slurry and an additive mixture
  • the present invention is directed to a dispersion composition comprising a cement-based sealing slurry comprising a) a Portland cement comprising an aluminate phase and b) a polymer dispersion and an additive mixture, as well as the use thereof.
  • additives may be added to aqueous slurries or powder dispersants or improving their workability, i.e. kneadability, spreadybility, sprayability, pumpability, or lowability.
  • Such admixtures are capable of preventing the formation of solid agglomerates and of dispersing the particles already present and those newly formed by hydration and in this way improving the workability.
  • This effect is utilized in the preparation of construction material compositions which contain e.g. hydraulic binders, such as cement, lime, gypsum, hemihydrate or anhydrite.
  • hydraulic binders such as cement, lime, gypsum, hemihydrate or anhydrite.
  • set control agents or retarders may be used as additives to delay the hydration reaction and improve the workability.
  • the retarders delay the hydration on-set by inhibiting the dissolution of the reactive cement components, in particular aluminates, and/or by masking the calcium ions thereby slowing down the hydration reaction.
  • DE 4217181 A1 discloses condensation products of melamine and glyoxylic acids as additives for hydraulic binders. For improving the flexibility and the waterproofness, polymer dispersions are being applied in cement-based sealing slurries.
  • the present invention therefore relates to a dispersion composition
  • a dispersion composition comprising A) a cement-based sealing slurry comprising a) a Portland cement comprising an aluminate phase, wherein the amount of alumina in form of Al 2 O 3 is at least 2 wt.-% of the total mass of the aluminate-containing cement as determined by means of X-ray fluorescence (XRF), b) a polymer dispersion comprising a (co)polymer selected from the group consisting of acrylic acid ester polymer, acrylic-styrene copolymer, styrene-butadiene-based copolymer, vinyl acetate polymer, and ethylene-vinyl acetate copolymer; and B) an additive mixture comprising i) a polyol having the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 6 - hydroxyalkyl, C 2
  • the Portland cement is an ordinary Portland cement comprising at least 3 wt.-% of aluminate types selected from the group consisting of C3A, C4AF, and mixtures thereof, and/or ess than 5 wt.-% of aluminate type CAC in form of CA, C2AS, CA2, and C12A7, and/or at least 3 wt.-% of CaSO 4 ⁇ x H 2 O, wherein x is selected from 0 to 1.5, and/or CaSO 4 ⁇ x H 2 O, wherein x is selected from 0 to 1.5, and Al 2 O 3 and wherein the weight ratio of the CaSO 4 ⁇ x H 2 O to the amount of Al 2 O 3 is from 1:3 to 4:1, preferably from 1:2 to 3:1.
  • the cement-based sealing slurry consists of the Portland cement and the polymer dispersion and comprises from 10 to 50 wt.-%, preferably from 20 to 45 wt.-%, of the polymer dispersion, based on the total weight of the cement-based sealing slurry.
  • the polymer dispersion is an aqueous polymer dispersion, preferably having a solid polymer content, determined according to DIN EN ISO 3251, from 20 to 70 wt.-%, more preferably from 30 to 65 wt.-%, and in particular from 40 to 60 wt.-%, based on the total weight of the aqueous polymer dispersion or a powder dispersion, preferably having a (co)polymer content from 60 to 95 wt.-%, more preferably from 70 to 90 wt.- %, based on the total weight of the powder dispersion.
  • the (co)polymer of the polymer dispersion has a Tg, calculated using the Fox equation , of -60 to 0 °C, preferably of -30 to -5 °C and/or the polymer dispersion comprises an acrylic-styrene copolymer.
  • the polyol has a molecular weight of less than 200 g/mol, preferably of less than 150 g/mol, more preferably of less than 100 g/mol and/or a C/O ratio of from less than 2 to more than 0.72, preferably from 1.5 to 0.8, in particular wherein the polyol is glycerol.
  • the polycondensate of glyoxylic acid is an amine-glyoxylic acid condensate, preferably wherein the amine-glyoxylic acid condensate is selected from the group consisting of a melamine-glyoxylic acid condensate, a urea-glyoxylic acid condensate, a melamine-urea-glyoxylic acid condensate, and a polyacrylamide-glyoxylic acid condensate, more preferably urea-glyoxylic acid condensate.
  • the carbonate source is selected from a group consisting of limestone, dolomite, calcium-magnesium carbonate, siderite, sodium carbonate, potassium carbonate, hydrogen carbonate, lithium carbonate, guanidinium carbonate, and calcium carbonate and/or wherein the carbonate source has a solubility in water of more than 0.08 g/l at 25 °C.
  • the salt of is present in the additive mixture and wherein R2 is H, R3 is C 3 -C 6 alkyl which may be substituted by 1 to 5 OH, and R4 is COOY, and Y is X being an alkali metal, preferably wherein the salt is sodium gluconate.
  • the weight ratio of the (co)polymer of the polymer dispersion to the Portland cement is from 2:1 to 1:2, preferably from 1.5:1 to 1:1.4, more preferably from 1.3:1 to 1: 1.2 and/or the weight ratio of water to the Portland cement is from 2:1 to 1:2, preferably from 1.5:1 to 1:1.4, more preferably from 1.3:1 to 1:1.2 and/or the weight ratio of the polymer dispersion to the Portland cement is from 4:1 to 1:1.3, preferably from 3:1 to 1:1, more preferably from 2.5:1 to 1: 1.1.
  • the dispersion composition further comprises C) calcium sulfate.
  • the present invention relates to the use of the dispersion composition according to the first aspect for improving flexibilisation or for providing waterproofness.
  • an additive mixture comprising i) a polyol having the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, -OH, C 1 -C 5 -alkyl, wherein o is an integer from 0-5, and/or ii) NR 1 R 2 R 3 , wherein R 1 is C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, (CH 2 O) n -OH, (CH 2 CH 2 O) n -OH, or (CH
  • AM-a additive mixture
  • the carbonate source is comprised in the additive mixture (AM-a).
  • the present invention relates to a flexible water-proofing membrane obtained from a dispersion composition according to the first aspect.
  • the present invention relates to method of sealing a concrete or masonry structure comprising applying to the concrete or masonry structure the dispersion composition according to the first aspect.
  • the terms “about” and “approximately” denote an interval of accuracy that a person skilled in the art will understand to still ensure the technical effect of the feature in question.
  • the term typically indicates a deviation from the indicated numerical value of ⁇ 20 %, preferably ⁇ 15 %, more preferably ⁇ 10 %, and even more preferably ⁇ 5 %.
  • the term “comprising” is not limiting.
  • the term “consisting of” is considered to be a preferred embodiment of the term “comprising of”. If hereinafter a group is defined to comprise at least a certain number of embodiments, this is meant to also encompass a group which preferably consists of these embodiments only.
  • first”, “second”, “third” or “(a)”, “(b)”, “(c)”, “(d)” etc. and the like in the description and in the claims, are used for distinguishing between similar elements and not necessarily for describing a sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances and that the embodiments of the invention described herein are capable of operation in other sequences than described or illustrated herein.
  • first, “second”, “third” or “(a)”, “(b)”, “(c)”, “(d)”, “i”, “ii” etc. relate to steps of a method or use or assay there is no time or time interval coherence between the steps, i.e.
  • substituted means that a hydrogen atom bonded to a designated atom is replaced with a specified substituent, provided that the substitution results in a stable or chemically feasible compound. Unless otherwise indicated, a substituted atom may have one or more substituents and each substituent is independently selected.
  • substituted when used in reference to a designated atom, means that attached to the atom is a hydrogen, which can be replaced with a suitable substituent.
  • the term “one or more” is intended to cover at least one substituent, e.g.1 to 10 substituents, preferably 1, 2, 3, 4, or 5 substituents, more preferably 1, 2, or 3 substituents, most preferably 1, or 2 substituents.
  • substituents e.g.1 to 10 substituents, preferably 1, 2, 3, 4, or 5 substituents, more preferably 1, 2, or 3 substituents, most preferably 1, or 2 substituents.
  • C n - C m indicates in each case the possible number of carbon atoms in the group.
  • halogen denotes in each case fluorine, bromine, chlorine or iodine, in particularluorine, chlorine, or bromine.
  • alkyl denotes in each case a straight-chain or branched alkyl group having usually from 1 to 6 carbon atoms, preferably 1 to 5 or 1 to 4 carbon atoms, more preferably 1 to 3 or 1 or 2 carbon atoms.
  • alkyl group examples include methyl, ethyl, n-propyl,so-propyl, n-butyl, 2-butyl, iso-butyl, tert-butyl, n-pentyl, 1-methylbutyl, 2-methylbutyl, 3-methylbutyl, 2,2-dimethylpropyl, 1-ethylpropyl, n-hexyl, 1,1-dimethylpropyl, 1,2-dimethylpropyl, 1-methylpentyl, 2-methylpentyl, 3-methylpentyl, 4-methylpentyl, 1,1-dimethylbutyl, 1,2- dimethylbutyl, 1,3-dimethylbutyl, 2,2-dimethylbutyl, 2,3-dimethylbutyl, 3,3-dimethylbutyl, 1- ethylbutyl, 2-ethylbutyl, 1,1,2-trimethylpropyl, 1,2,2-trimethylpropyl, 1-ethyl
  • alkoxy denotes in each case a straight-chain or branched alkyl group which is bonded via an oxygen atom and has usually from 1 to 6 carbon atoms, preferably 1 to 2 carbon atoms, more preferably 1 carbon atom.
  • alkoxy group examples are methoxy, ethoxy, n-propoxy, iso-propoxy, n-butyloxy, 2-butyloxy, iso-butyloxy, tert.-butyloxy, and the like.
  • hydroxyalkyl denotes in each case a straight-chain or branched alkyl group having usually from 1 to 6 carbon atoms and being further substituted with 1 to 5, preferably with 1 to 2 hydroxy groups, in particular with 1 hydroxy group.
  • the one hydroxy group is terminating the straight-chain or branched alkyl group so that the hydroxy group is bonded to an alkyl bridge, which is bonded to the remainder of the molecule.
  • hydroxyalkenyl denotes in each case an unsaturated hydrocarbon group having usually 2 to 6, preferably 2 to 4 carbon atoms comprising at least one carbon- carbon double bond in any position and being further substituted with 1 to 5, preferably with 1 to 2 hydroxy groups, in particular with 1 hydroxy group.
  • the one hydroxy group iserminating the unsaturated hydrocarbon group so that the hydroxy group is bonded to an alkenyl bridge, which is bonded to the remainder of the molecule.
  • Examples of an hydroxyalkenyl are hydroxyvinyl, hydroxyallyl, hydroxymethallyl, hydroxybuten-1-yl, 2-hydroxy- 2-penten-1-yl, 1-hydroxy-3-penten-1-yl and the like.
  • aminoalkyl denotes in each case a straight-chain or branched alkyl group having usually from 1 to 6 carbon atoms and being further substituted with 1 to 5, preferably with 1 to 2 amino groups, in particular 1 amino group.
  • the one amino group is terminating the straight-chain or branched alkyl group so that the amino group is bonded to an alkyl bridge, which is bonded to the remainder of the molecule.
  • aminoalkyl group examples include aminomethyl, aminoethyl, n-aminopropyl, 2-aminopropyl, n-aminobutyl, 2- aminobutyl, 2-amino-2-methylpropyl, n-aminopentyl, and n-aminohexyl.
  • Aminomethyl, aminoethyl, aminopropyl, and aminobutyl, are preferred, in particular aminoethyl.
  • heterocyclic or “heterocyclyl” includes, unless otherwise indicated, in general a 5- or 6-membered, in particular 6-membered monocyclic ring.
  • the heterocycle may be saturated, partially or fully unsaturated, or aromatic, wherein saturated means that only single bonds are present, and partially or fully unsaturated means that one or more double bonds may be present in suitable positions, while the Hückel rule for aromaticity is not fulfilled, whereas aromatic means that the Hückel (4n + 2) rule is fulfilled.
  • the heterocycle typically comprises one or more, e.g.1, 2, 3, or 4, preferably 1, 2, or 3 heteroatoms selected from N, O and S as ring members, where S-atoms as ring members may be present as S, SO or SO 2 .
  • the remaining ring members are carbon atoms.
  • the heterocycle is an aromatic heterocycle, preferably a 5- or 6-membered aromatic heterocycle comprising one or more, e.g.1, 2, 3, or 4, preferably 1, 2, or 3 heteroatoms selected from N, O and S as ring members, where S-atoms as ring members may be present as S, SO or SO 2 .
  • aromatic heterocycles are provided below in connection with the definition of “hetaryl”. “Hetaryls” or “heteroaryls” are covered by the term “heterocycles”.
  • the saturated or partially or fully unsaturated heterocycles usually comprise 1, 2, 3, 4 or 5, preferably 1, 2 or 3 heteroatoms selected from N, O and S as ring members, where S-atoms as ring members may be present as S, SO or SO 2 .
  • S, SO or SO 2 is to be understood as follows: When referring to compositions and the weight percent of the therein comprised ingredients it is to be understood that according to the present invention the overall amount of ingredients does not exceed 100% ( ⁇ 1% due to rounding).
  • Preferred embodiment regarding the dispersion composition as well as the use thereof for improving flexibilisation or for providing waterproofness, a flexible water-proofing membrane obtained from said dispersion composition and a method of sealing a concrete or masonry structure are described hereinafter.
  • the present invention relates in one embodiment to a dispersion composition
  • a dispersion composition comprising A) a cement-based sealing slurry comprising a) a Portland cement comprising an aluminate phase, wherein the amount of alumina in form of Al 2 O 3 is at least 2 wt.-% of the total mass of the aluminate-containing cement as determined by means of X-ray fluorescence (XRF), b) a polymer dispersion comprising a (co)polymer selected from the group consisting of acrylic acid ester polymer, acrylic-styrene copolymer, styrene-butadiene-based copolymer, vinyl acetate polymer, and ethylene-vinyl acetate copolymer; and B) an additive mixture comprising A) a cement-based sealing slurry comprising a) a Portland cement comprising an aluminate phase, wherein the amount of alumina in form of Al 2 O 3 is at least 2
  • the dispersion compositions according to the present invention especially benefit from specific advantageous in term of drying properties. Without being bound to any theory, it is assumed that the herein disclosed additive mixture provides a controlled aluminate reaction, which results in a faster drying of the cement-based sealing slurry due to hydration.
  • the dispersion composition which are relevant for all aspects of the invention, are described in further detail hereinafter. It is to be understood that each preferred embodiment is relevant on its own as well as in combination with other preferred embodiments.
  • the mineralogical phases are indicated by their usual name followed by their cement notation.
  • the primary compounds are represented in the cement notation by the oxide varieties: C for CaO, S for SiO 2 , A for Al 2 O 3 , $ for SO 3 , H for H 2 O; this notation is used throughout.
  • the term "Portland cement” generally denotes any cement compound containing Portland clinker, especially CEM I, II, III, IV and V within the meaning of standard EN 197-1, paragraph 5.2.
  • a preferred cement is ordinary Portland cement (OPC) according to DIN EN 197-1 which may either contain calcium sulfate ( ⁇ 7% by weight) or is essentially free of calcium sulfate ( ⁇ 1% by weight).
  • Calcium aluminate cement (also referred to as CAC or high aluminate cement) means a cement containing calcium aluminate phases.
  • aluminate phase denotes any mineralogical phase resulting from the combination of aluminate (of chemical formula Al 2 O 3 , or "A” in cement notation), with other mineral species.
  • the amount of alumina (in form of Al 2 O 3 ) is at least 2 wt.-%, preferably at least 3 wt.-%, and more preferably at least 4 wt.-%, of the total mass of the aluminate-containing cement as determined by means of X-ray fluorescence (XRF).
  • XRF X-ray fluorescence
  • said mineralogical phase of aluminate type comprises e.g. tricalcium aluminate (C 3 A), monocalcium aluminate (CA), calcium-di-aluminate (CA2), mayenite (C 12 A 7 ), gehlenite (C2AS), tetracalcium aluminoferrite (C 4 AF), or a combination of several of these phases.
  • Sulfoaluminate cement has a content of yeelimite (of chemical formula 4CaO.3Al 2 O 3 .SO 3 or C 4 A 3 $ in cement notation) of greater than 15% by weight.
  • Mineralogical phases in cement are typically determined using quantitative X-ray diffraction (XRD).
  • the Portland cement is an ordinary Portland cement.
  • the ordinary Portland cement comprises aluminate types selected from the group consisting of C3A, C4AF, and mixtures thereof.
  • the ordinary Portland cement comprises at least 1 wt.-%, more preferably at least 2 wt.-%, and even more preferably at least 3 wt.-%, of aluminate types selected from the group consisting of C3A, C4AF, and mixtures thereof.
  • the ordinary Portland cement comprises less than 5 wt.-%, more preferably less than 4 wt.-%, and even more preferably less than 3 wt.-%, of aluminate type CAC in form of CA, C2AS, CA2, and C12A7.
  • the ordinary Portland cement according to the present invention contains an aluminate phase and may additionally contain at least one sulfate source, preferably calcium sulfate source.
  • the calcium sulfate source may be selected from calcium sulfate dihydrate, anhydrite, ⁇ - and ⁇ -hemihydrate, i.e. ⁇ -bassanite and ⁇ -bassanite, or mixtures thereof.
  • the calcium sulfate is ⁇ -bassanite and/or ⁇ -bassanite.
  • the ordinary Portland cement comprises at least 3 wt.-%, more preferably at least 4 wt.-%, and even more preferably at least 5 wt.-%, of CaSO 4 ⁇ x H 2 O, wherein x is selected from 0 to 1.5. It is further preferred, that the ordinary Portland cement comprises from at least 3 to less than 7 wt.-%, more preferably from at least 4 to 6 wt.-%, and even more preferably 4.5. to 5.5 wt.-%, of CaSO 4 ⁇ x H 2 O, wherein x is selected from 0 to 1.5.
  • the C3A, C4AF, CA, C2AS, CA2, C12A7, and CaSO 4 ⁇ x H 2 O are determined using quantitative X-ray diffraction (XRD).
  • XRD quantitative X-ray diffraction
  • the ordinary Portland cement comprises at least 5 wt.-%, more preferably at least 10 wt.-%, and even more preferably at least 15 wt.-%, of sulfoaluminate types such as yeelimite having the chemical formula 4CaO.3Al 2 O 3 .SO 3 or C 4 A 3 $ in cement notation.
  • the ordinary Portland cement comprises CaSO 4 ⁇ x H 2 O, wherein x is selected from 0 to 1.5, and Al 2 O 3 and wherein the weight ratio of the CaSO 4 ⁇ x H 2 O to the amount of Al 2 O 3 is from 1:3 to 4:1, preferably from 1:2 to 3:1.
  • the cement-based sealing slurry consists of the Portland cement and the polymer dispersion. In this connection it is preferred that the cement-based sealing slurry comprises from 10 to 50 wt.-%, preferably from 15 to 48 wt.-%, and more preferably from 20 to 45 wt.-%, of the polymer dispersion, based on the total weight of the cement-based sealing slurry.
  • the cement-based sealing slurry comprises from 50 to 90 wt.-%, preferably from 52 to 85 wt.-%, and more preferably from 55 to 80 wt.-%, of the Portland cement, based on the total weight of the cement-based sealing slurry.
  • the polymer dispersion comprising a (co)polymer selected from the group consisting of acrylic acid ester polymer, acrylic-styrene copolymer, styrene-butadiene-based copolymer, vinyl acetate polymer, and ethylene-vinyl acetate copolymer, preferably selected from the group consisting of acrylic acid ester polymer and acrylic-styrene copolymer.
  • the polymer dispersion is an aqueous polymer dispersion.
  • the (co)polymer of the polymer dispersion is preferably made up of ethylenically unsaturated compounds in polymerized form.
  • the preparation of these polyaddition compounds is generally carried out by metal complex-catalyzed, anionically catalyzed, cationically catalyzed and particularly preferably free-radically catalyzed polymerization, as is familiar to a person skilled in the art, of ethylenically unsaturated compounds.
  • the free-radically catalyzed polymerization of ethylenically unsaturated compounds will be familiar to a person skilled in the art and is, in particular, carried out by the method of free- radical bulk, emulsion, solution, precipitation, or suspension polymerization, with free-radically initiated aqueous emulsion polymerization being particularly preferred.
  • Carrying out free-radically initiated emulsion polymerization of ethylenically unsaturated compounds (monomers) in an aqueous medium is known [cf. Emulsion polymerization in Encyclopedia of Polymer Science and Engineering, Vol.8, pages 659 ff. (1987); D. C. Blackley, in High Polymer Latices, Vol.1, pages 35 ff. (1966); H.
  • Free-radically initiated aqueous emulsion polymerization is usually carried out by dispersing the monomers, generally with concomitant use of dispersants such as emulsifiers and/or protective colloids, in an aqueous medium and polymerizing them by means of at least one water-soluble free-radical polymerization initiator.
  • the residual contents of unreacted monomers in the aqueous polymer dispersions obtained are decreased by chemical and/or physical after-treatment, the polymer solids content is set to a desired value by dilution or concentration or further customary additives, for example foam- or viscosity-modifying additives, are added to the aqueous polymer dispersion.
  • customary additives for example foam- or viscosity-modifying additives
  • Possible monomers are, in particular, monomers which can be free-radically polymerized in a simple manner, for example ethylene, vinylaromatic monomers such as styrene, ⁇ - methylstyrene, or o-chlorostyrene, vinyl acetate, acrylic acid, esters of acrylic acid and methacrylic acid with alkanols, which generally have from 1 to 12, preferably from 1 to 8 and in particular from 1 to 4, carbon atoms, especially methyl, ethyl, n-butyl, isobutyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl (e.g.
  • esters of acrylic acid and methacrylic acid with alkanes which generally have from 1 to 12, preferably from 1 to 10, and in particular from 1 to 8, carbon atoms (e.g. ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, 2- propylheptyl acrylate), and 1,3-butadiene.
  • the polymer dispersion comprises an acrylic-styrene copolymer.
  • the acrylic-styrene copolymer is obtainable by free-radical polymerization of styrene and/or methylstyrene, in particular styrene, with acrylates selected from the group consisting of methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, hydroxyethylmethacrylate, 2-propylheptyl acrylate, and mixtures thereof, in particular selected from the group consisting of 2-ethylhexyl acrylate, hydroxyethylmethacrylate, butyl acrylate, and mixtures thereof.
  • methylstyrene refers to alpha-methylstyrene, beta- methylstyrene, 2-methylstyrene, 3-methylstyrene, and 4-methylstyrene, preferably to alpha- methylstyrene.
  • the acrylic-styrene copolymer is obtainable by free-radical polymerization of 15 to 50 wt.-%, more preferably 20 to 45 wt.-%, and in particular 25 to 40 wt.-%, of styrene and/or methylstyrene with 50 to 85 wt.-%, more preferably 55 to 80 wt.-%, and in particular 60 to 75 wt.-%, of at least one acrylate.
  • styrene is polymerized with the at least one acrylate selected from the group consisting of methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, hydroxyethylmethacrylate, 2-propylheptyl acrylate, and mixtures thereof, in particular selected from the group consisting of 2-ethylhexyl acrylate, hydroxyethylmethacrylate, butyl acrylate, and mixtures thereof.
  • the polymer dispersion comprises a styrene-butadiene-based copolymer.
  • the polymer dispersion comprises a vinyl acetate polymer.
  • the polymer dispersion further comprises a terpolymer.
  • Suitable erpolymers are addition products of vinyl acetate, ethylene and vinyl ester.
  • the vinyl esters are those of carboxylic acids having 1 to 15 carbon atoms.
  • the polymer dispersion is an aqueous polymer dispersion, preferably having a solid polymer content, determined according to DIN EN ISO 3251, from 20 to 70 wt.-%, more preferably from 25 to 72 wt.-%, even more preferably from 30 to 65 wt.-%, and in particular from 40 to 60 wt.-%, based on the total weight of the aqueous polymer dispersion.
  • the polymer dispersion is a powder dispersion, preferably having a (co)polymer content from 60 to 95 wt.-%, more preferably from 65 to 92 wt.-%, even more preferably from 70 to 90 wt.-%, based on the total weight of the powder dispersion.
  • the (co)polymer of the polymer dispersion has a Tg, calculated using the Fox equation, of -60 to 0 °C, preferably of -50 to -4 °C, more preferably of -40 to -2 °C, even more preferably of -30 to -5 °C. According to Fox (cf. T.G. Fox, Bull. Am. Phys. Soc.
  • Tg of polymer dispersions wherein X 1 , X 2, ..., X n are the mass fractions 1, 2, ..., n and Tg 1 , Tg 2, , ..., Tg n are the glass ransition temperatures, in kelvins, of homopolymers of each of the monomers 1, 2, ..., n.
  • the individual Tgs are known, for example, from Ullmann's Encyclopedia of Industrial Chemistry, VCH, Weinheim, Vol. A 21 (1992) p.169 and from J. Brandrup, E.
  • the (co)polymers of the polymer dispersion are preferably present in the form of particles having an average particle diameter of from 10 to 1000 nm, more preferably from 30 to 600 nm, and in particular from 50 to 400 nm, measured by the pseudoelastic light scattering method (ISO standard 13321; cumulant z-average).
  • the aqueous polymer dispersion may additionally comprises at least one surface active compound.
  • the surface active compound serves to stabilize the aqueous dispersion of the polymer by keeping the particles of the polymer dispersed.
  • the surface active compound may be an emulsifier, a protective colloid or a mixture of both of them.
  • the emulsifier and the protective colloid are distinct from each other by their weight-average molar mass Mw.
  • An emulsifier has typically a weight average molar mass Mw in general below 2000, while the weight-average molar mass Mw of the protective colloid may be up to 50000, in particular from above 2000 to up to 50000.
  • the amount of the surface active compound is in the range from 0.1 to 10% by weight, in particular in the range from 0.5 to 5% by weight, based on the total amount of polymer in the aqueous polymer dispersion.
  • the surface active compound comprises one or more emulsifiers.
  • the emulsifier is non-ionic, anionic, or cationic.
  • an anionic emulsifier is compatible with another anionic emulsifier or a non-ionic emulsifier.
  • a cationic emulsifier is typically compatible with another cationic emulsifier or a non- ionic emulsifier.
  • the emulsifier is an anionic emulsifier, a combination of two or more anionic emulsifier or a combination of at least one anionic emulsifier and at least one non-ionic emulsifier.
  • Examples of customary nonionic emulsifiers are the Emulgin B grades (cetyl/stearyl alcohol ethoxylates, RTM BASF), Dehydrol LS grades (fatty alcohol ethoxylates, EO units: 1-10, RTM BASF), Lutensol A grades (C 12 C 14 -fatty alcohol ethoxylates, EO units: 3-8, RTM BASF), Lutensol AO grades (C 13 C 15 -oxo alcohol ethoxylates, EO units: 3-30), Lutensol AT grades (C 16 C 18 -fatty alcohol ethoxylates, EO units: 11-80), Lutensol ON grades (C10-oxo alcohol ethoxylates, EO units: 3-11) and Lutensol TO grades (C 13 -oxo alcohol ethoxylates, EO units: 3-20).
  • Emulgin B grades cetyl/stearyl alcohol ethoxylates, RTM BASF
  • EO units means the number average of ethylene oxide repeating units in the emulsifier.
  • Anionic emulsifiers include for example the alkali metal salts of dialkyl esters of sulfosuccinic acid, the alkali metal salts and the ammonium salt of C 8 -C 12 alkyl sulfates, the alkali metal salts and the ammonium salts of C 12 -C 18 alkylsulfonic acids, the alkali metal salts and the ammonium salts of C 9 -C 18 alkylarylsulfonic acid, the alkali metal salts and the ammonium salts of sulfuric acid monoesters of ethoxylated C 12 -C 18 alkanols (EO units: 4-30) or a sulfuric acid monoester of an ethoxylated (C 4 -C 12 alkyl)phenol (EO units: 3-50).
  • emulsifiers are fatty alcohol phosphates, alkylphenol phosphates, alkyl polyglycol ether phosphates, alkyl polyalkylene oxide phosphates, and fatty alcohol ether phosphates and the salts thereof, in particular the alkalimetal salts and ammonium salts thereof, with particular preference given to the alkalimetal salts such as sodium salts.
  • suitable emulsifiers may be found in Houben-Weyl, Methoden der organischen Chemie, volume XIV/1, Makromolekulare Stoffe, Georg-Thieme-Verlag, Stuttgart, 1961, pages 192 to 208.
  • suitable protective colloids may be non-ionic, anionic or cationic.
  • protective colloids are poly(vinyl alcohols), poly(alkylene glycols), poly(acrylic acids) and the alkali metal salt thereof, poly(methacrylic acids) and the alkali metal salt thereof and gelatin derivatives.
  • Anionic protective colloid can also be a copolymer, containing a suitable amount of at least one anionic monomer, such as acrylic acid, methacrylic acid, maleic acid, 2-acrylamido-2-methylpropane sulfonic acid, para-vinylphenyl sulfonic acid or salt forms thereof, preferably alkali metal salts thereof, in polymerized form.
  • cationic protective colloids are homo polymers and copolymers containing a sufficient amount of cationic monomers, in particular monoethylenically unsaturated monomers having one or more amino groups, which are N-protonated or N-alkylated.
  • Examples include N-protonated and N- alkylated derivatives of homopolymers or copolymers of N-vinylformamide in their at least partly hydrolyzed form, homopolymers or copolymers of N-vinylacetamide in their at least partly hydrolyzed form, N-protonated and N-alkylated derivatives of homopolymers or copolymers of N-vinylcarbazole, N-protonated and N-alkylated derivatives of homopolymers or copolymers of 1-vinylimidazole, N-protonated and N-alkylated derivatives of homopolymers or copolymers of 2-vinylimidazole, N-protonated and N-alkylated derivatives of homopolymers or copolymers of 2-vinylpyridine, N-protonated and N-alkylated derivatives of homopolymers or copolymers of 4- vinylpyridine, N-protonated and N-al
  • cationic protective colloids may be acrylamide, methacrylamide and N-vinyl pyrrolidone.
  • the protective colloids are distinct from the polymers dispersed in the aqueous polymer dispersion as they are water-soluble or water dispersible.
  • water-soluble or water dispersible is understood that the corresponding protective colloid can be dissolved or dispersed in deionized water at 20°C and 1013 mbar in an amount of at least 10 g/L polymer such that the resulting aqueous solution has either no measurable particle size or a particle size of at most 20 nm as determined by dynamic light scattering in accordance with DIN 22412:2008.
  • the polyol has the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 3 -hydroxyalkyl, C 2 -C 3 -hydroxyalkenyl, C 1 -C 3 -aminoalkyl, -OH, C 1 -C 3 -alkyl, wherein o is an integer from 0-5, more preferably R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 2 -hydroxyalkyl, or -OH, wherein o is an integer from 0-5.
  • the polyol has a molecular weight of less than 200 g/mol, preferably of less than 150 g/mol, and more preferably of less than 100 g/mol. It is further preferred that the polyol has a molecular weight of 80 to less than 200 g/mol, preferably of 83 to less than 150 g/mol, and more preferably of 85 to less than 100 g/mol. In a preferred embodiment, the polyol has a C/O ratio of from less than 2 to more than 0.72, preferably from 1.5 to 0.8 and more preferably from 1.1 to 0.9.
  • the polyol is selected from the group consisting of ethylene glycol, glycerol, pentaerythritol, and C 4 -C 7 sugar alcohols such as erythritol, threitol, arabitol, xylitol, ribitol, mannitol, sorbitol, galactitol, fucitol, iditol, inositol, and volemitol, in particular wherein the polyol is glycerol.
  • R 1 to R 3 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 - hydroxyalkenyl, C 1 -C 6 -aminoalkyl, (CH 2 O) n -OH, (CH 2 CH 2 O) n -OH, or (CH 2 CH 2 CH 2 O) n -OH, wherein n is an integer from 1 to 10, preferably from 1 to 5, more preferably from 1 to 3.
  • R 1 to R 3 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 - hydroxyalkenyl, (CH 2 O) n -OH, (CH 2 CH 2 O) n -OH, or (CH 2 CH 2 CH 2 O) n -OH, wherein n is an integer from 1 to 10, preferably from 1 to 5, more preferably from 1 to 3.
  • R 1 to R 3 are independently C 1 -C 6 -hydroxyalkyl.
  • R 1 to R 3 are the same.
  • R 1 to R 3 are independently selected from the group consisting of hydroxymethyl, hydroxyethyl, n-hydroxypropyl, 2-hydroxypropyl, n-hydroxybutyl, 2- hydroxybutyl, 2-hydroxy-2-methylpropyl, n-hydroxypentyl, and n-hydroxyhexyl, preferably selected from the group consisting of hydroxymethyl, hydroxyethyl, hydroxypropyl, and hydroxybutyl, in particular hydroxyethyl.
  • Glyoxylic acid has the following structure:
  • addition products of glyoxylic acid refer to products, which are obtainable by reacting a nucleophilic compound with the ⁇ -carbonyl group of glyoxylic acid, so as to obtain ⁇ - substituted ⁇ -hydroxy- acetic acid or a salt thereof as an adduct.
  • condensation products of glyoxylic acid refer to condensation products obtainable by reacting a compound containing at least one amino or amido group with the ⁇ - carbonyl group of glyoxylic acid, such that water is set free.
  • the dispersion composition comprises the polycondensate of glyoxylic acid.
  • the polycondensate of glyoxylic acid is an amine-glyoxylic acid condensate.
  • amine-glyoxylic acid condensate as used herein is intended to mean a condensate of glyoxylic acid with a compound containing amino or amido groups reactive with aldehydes.
  • Examples of compounds containing aldehyde-reactive amino or amido groups include urea, thiourea, melamine, guanidine, acetoguanamine, benzoguanamine and other acylguanamines and polyacrylamide.
  • the amine-glyoxylic acid condensate is selected from the group consisting of a melamine-glyoxylic acid condensate, a urea-glyoxylic acid condensate, a melamine-urea-glyoxylic acid condensate, and a polyacrylamide-glyoxylic acid condensate, more preferably urea-glyoxylic acid condensate.
  • the amine-glyoxylic acid condensates are obtainable by reacting glyoxylic acid with a compound containing aldehyde-reactive amino or amido groups.
  • the glyoxylic acid can be used as an aqueous solution or as glyoxylic acid salts, preferably glyoxylic acid alkaline metal salts.
  • the amine compound can be used as salt, for example as guanidinium salts.
  • the amine compound and the glyoxylic acid are reacted in a molar ratio of 0.5 to 2 equivalents, preferably 1 to 1.3 equivalents, of glyoxylic acid per aldehyde-reactive amino or amido group.
  • the reaction is carried out at a temperature of 0 to 120 °C, preferably 25 to 105 °C, most preferably 50 to 105 °C.
  • the pH value is preferably from 0 to 8.
  • the viscous products obtained in the reaction can be used as such, adjusted to a desired solids content by dilution or concentration or evaporated to dryness by, e.g., spray-drying, drum-drying, or flash-drying.
  • the amine-glyoxylic acid condensates have molecular weights in the range of from 500 to 25000 g/mol, preferably 1000 to 10000 g/mol, particularly preferred 1000 to 5000 g/mol.
  • the dispersion composition comprises the sulfite addition product of glyoxylic acid.
  • the sulfite addition product has the following formula: wherein X is in each case independently selected from H or a cation equivalent K a , wherein K is an alkali metal, alkaline earth metal, zinc, iron, aluminum, ammonium, or a phosphonium cat ion, and wherein a is 1/n, wherein n is the valence of the cation. More preferably, X is H or Ka, wherein K is an alkali metal.
  • K is lithium, sodium or potassium. It is to be understood that also mixed salts are possible.
  • X is independently sodium or potassium or a mixture thereof.
  • the carbonate source may be an inorganic carbonate having an aqueous solubility of 0.1 g/l or more. The aqueous solubility of the inorganic carbonate is determined in water (starting at pH 7) at 25 °C. These characteristics are well known to those skilled in the art.
  • the inorganic carbonate may be selected from alkaline metal carbonates such as potassium carbonate, sodium carbonate or lithium carbonate, and alkaline earth metal carbonates satisfying the required aqueous solubility, such as magnesium carbonate.
  • the carbonate source is selected from organic carbonates.
  • Organic carbonate denotes an ester of carbonic acid.
  • the organic carbonate is hydrolyzed in the presence of the cementitious system to release carbonate ions.
  • the organic carbonate is selected from ethylene carbonate, propylene carbonate, glycerol carbonate, dimethyl carbonate, di(hydroxyethyl)carbonate or a mixture thereof, preferably ethylene carbonate, propylene carbonate, and glycerol carbonate or a mixture thereof, and in particular ethylene carbonate and/or propylene carbonate.
  • the carbonate source is selected from a group consisting of limestone, dolomite, calcium-magnesium carbonate, siderite, sodium carbonate, potassium carbonate, hydrogen carbonate, lithium carbonate, guanidinium carbonate, and calcium carbonate.
  • the carbonate source has a solubility in water of more than 0.08 g/l, more preferably of more than 0.09 g/l, and in particular of more than 0.1 g/l, at 25 °C.
  • the salt is sodium gluconate.
  • the additive mixture comprising i) a polyol having the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 6 - hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, -OH, C 1 -C 5 -alkyl, wherein o is an integer rom 0-5 and ii) NR 1 R 2 R 3 , wherein R 1 is C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, (CH 2 O) n -OH, (CH 2 CH 2 O) n - OH, or (CH 2 CH 2 CH 2 O) n -OH; R 2 and R 3 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl,
  • the additive mixture comprises components i) to iv).
  • the weight ratio of the (co)polymer of the polymer dispersion to the Portland cement is from 2:1 to 1:2, preferably from 1.5:1 to 1:1.4, more preferably from 1.3:1 to 1: 1.2.
  • the weight ratio of water to the Portland cement is from 2:1 to 1:2, preferably from 1.5:1 to 1:1.4, more preferably from 1.3:1 to 1:1.2.
  • the weight ratio of the polymer dispersion to the Portland cement is from 4:1 to 1:1.3, preferably from 3:1 to 1:1, more preferably from 2.5:1 to 1: 1.1.
  • the dispersion composition comprises the cement-based sealing slurry from 50 to 99 wt.-%, more preferably from 70 to 99 wt.-%, and in particular from 80 to 99 wt.-%, and the additive mixture from 1 to 50 wt.-%, more preferably from 1 to 30 wt.-%, and in particular from 1 to 20 wt.-%, each based on the total amount of the dispersion composition.
  • the dispersion composition further comprises C) calcium sulfate.
  • the dispersion composition further comprises D) at least one additional retarder.
  • the at least one additional retarder may be selected from the group consisting of: -The bisulfite adduct as synthesized according to WO2017/212045A1: additive 1, page 26; the resulting suspension can be used directly or can be present as a powder which is obtainable, e.g., by drum-drying, spray drying, or flash-drying; -Fruit acids (citric acid, tartaric acid, gluconic acid) or salts thereof; - ⁇ -hydroxy carboxylic acids or salts thereof; and -Organic phosphates, phosphonoalkylcarboxylic acids, phosphonates (such as ATMP, BHMTMP, DTPMP, EDTMP, HDTMP, HEDP, HEMPA, and PBTC as provided by Zschimmer & Schwarz).
  • the dispersion composition further comprises E) at least one additional accelerator.
  • the at least one additional accelerator may be selected from the group consisting of: -Water-soluble organic carbonates such as ethylene carbonate, propylene carbonate, trimethylene carbonate, glycerol carbonate, dimethyl carbonate, or di(hydroxyethyl)carbonate, inorganic carbonates, such as alkali metal carbonates, like sodium carbonate; -Calcium-silicate-hydrate nanocrystals in suspension or as powders as described in WO2010/026155A1, EP14198721, WO2014/114784 or WO2014/114782; -Amorphous aluminum hydroxide (e.g.
  • the dispersion composition further comprises F) at least one dispersant.
  • the dispersant is preferably a polymeric dispersant, which has anionic and/or anionogenic groups and polyether side chains, which preferably comprise polyalkylene glycol side chains. The anionic and/or anionogenic groups and the polyether side chains are preferably attached to the backbone of the polymeric dispersant.
  • the dispersants are in this case more preferably selected from the group of polycarboxylate ethers (PCEs), the anionic group being in the case of PCEs carboxylic groups and/or carboxylate groups, and phosphorylated polycondensates. Most preferable are the polycarboxylate ethers (PCEs).
  • the PCE is preferably produced by the radical copolymerization of a polyether macromonomer and an acid monomer in a way that at least 45 mol-%, preferably at least 80 mol-% of all structural units of the copolymer were formed by copolymerization of the polyether macromonomer and the acid monomer.
  • acid monomer means in particular a monomer comprising anionic and/or anionogenic groups.
  • polyether macromonomer means in particular a monomer comprising at least two ether groups, preferably at least two alkylene glycol groups.
  • the polymeric dispersant preferably comprises as anionic and/or anionogenic group at least one structural unit of the general formulae (la), (lb), (lc) and/or (Id):
  • R 1 is H or an unbranched or branched C 1 -C 4 alkyl group, CH 2 COOH or CH 2 CO-X-R 3 ;
  • R 2 is OM, PO 3 M 2 , or O-PO 3 M 2 ; with the proviso that X is a chemical bond if R 2 is OM; R 3 is PO 3 M 2 , or O-PO 3 M 2 ;
  • R 3 is H or an unbranched or branched C 1 -C 4 alkyl group; n is 0, 1, 2, 3 or 4;
  • R 4 is PO 3 M 2 , or O-PO 3 M 2 ; (lc) in which
  • R 5 is H or an unbranched or branched C 1 -C 4 alkyl group
  • Z is O or NR 7 ;
  • R 7 is H, (C n H 2n )-OH, (C n H 2n )-PO 3 M 2 , (C n H 2n )-OPO 3 M 2 , (C 6 H 4 )-PO 3 M 2 , or (C 6 H 4 )-OPO 3 M 2 , and n is 1 , 2, 3 or 4;
  • R 6 is H or an unbranched or branched C 1 -C 4 alkyl group
  • Q is NR 7 or O
  • R 7 is H, (C n H 2n )-OH, (C n H 2n )-PO 3 M 2 , (C n H 2n )-OPO 3 M 2 , (C 6 H 4 )-PO 3 M 2 , or (C 6 H 4 )-OPO 3 M 2 ; n is 1 , 2, 3 or 4; and where each M in the above formulae independently of any other is H or a cation equivalent.
  • polymeric dispersant comprises as polyether side chain at least one structural unit of the general formulae (I la), (lib), (lie) and/or (lid):
  • R 10 , R 11 and R 12 independently of one another are H or an unbranched or branched C 1 -C 4 alkyl group;
  • Z is O or S;
  • E is an unbranched or branched C 1 -C 6 alkylene group, a cyclohexylene group, CH 2 - C 6 H 10 , 1,2-phenylene, 1,3-phenylene or 1,4-phenylene;
  • G is O, NH or CO-NH; or E and G together are a chemical bond;
  • A is an unbranched or branched alkylene with 2, 3, 4 or 5 carbon atoms or CH 2 CH(C 6 H 5 );
  • n is 0, 1, 2, 3, 4 or 5;
  • a is an integer from 2 to 350;
  • R 13 is H, an unbranched or branched C 1 -C 4 alkyl group, CO-NH 2 or COCH 3 ;
  • the polymeric dispersant is a phosphorylated polycondensation product comprising structural units (III) and (IV): (III) in which T is a substituted or unsubstituted phenyl or naphthyl radical or a substituted or unsubstituted heteroaromatic radical having 5 to 10 ring atoms, of which 1 or 2 atoms are heteroatoms selected from N, O and S; n is 1 or 2; B is N, NH or O, with the proviso that n is 2 if B is N and with the proviso that n is 1 if B is NH or O; A is an unbranched or branched alkylene with 2 to 5 carbon atoms or CH 2 CH(C 6 H 5 ); a is an integer from 1 to 300; R 25 is H, a branched or unbranched C 1 to C 10 alkyl radical, C 5 to C 8 cycloalkyl radical, aryl radical, or heteroaryl radical having 5 to 10
  • the polymeric dispersants comprising structural units (I) and (II) can be prepared by conventional methods, for example by free radical polymerization.
  • the preparation of the dispersants is, for example, described in EP0894811, EP1851256, EP2463314, and EP0753488.
  • the dispersant is a polymer comprising a sulfonic acid and/or sulfonate group.
  • the polymeric dispersant comprising sulfonic acids and/or sulfonates and is selected from the group consisting of lignosulfonates (LGS), melamine formaldehyde sulfonate condensates (MFS), ⁇ -naphthalene sulfonic acid condensates (BNS), sulfonated ketone-formaldehyde-condensates, and copolymers comprising sulfo group containing units and/or sulfonate group-containing units and carboxylic acid and/or carboxylate group-containing units.
  • LGS lignosulfonates
  • MFS melamine formaldehyde sulfonate condensates
  • BNS ⁇ -naphthalene sulfonic acid condensates
  • copolymers comprising sulfo group containing units and/or sulfonate group-containing units and carboxylic acid and/or carboxylate group-containing units
  • the lignosulfonates used as polymeric sulfonated dispersants are products, which are obtained as by-products of the paper industry. Such products are described in Ullmann's Encyclopedia of Industrial Chemistry, 5th Ed., Vol. A8, pages 586, 587. They comprise units of the strongly simplified and idealized formula wherein n is usually 5 to 500. Lignosulfonates have usually molecular weights between 2.000 and 100.000 g/mol. Generally, they are present in the form of their sodium-, calcium-, and/or magnesium salts. Examples for suitable lignosulfonates are the products marketed under the trade name Borresperse of the Norwegian company Borregaard LignoTech.
  • melamine-formaldehyde-sulfonate condensates also called MFS-resins
  • MFS-resins melamine-formaldehyde-sulfonate condensates
  • Preferred melamine-formaldehyde-sulfonate condensates comprise (strongly simplified and idealized) units of the formula Melamine formaldehyde sulfite (PMS) wherein n is typically a number from 10 to 300.
  • the molecular weight is preferably in the region from 2.500 to 80.000 g/mol.
  • An example for melamine-formaldehyde-sulfonate condensates are products marketed by the company BASF Construction Additives GmbH under the trade name Melment ® .
  • additional monomers can be co-condensated. In particular urea is suitable.
  • aromatic building units like gallic acid, aminobenzene sulfonic acid, sulfanilic acid, phenol sulfonic acid, aniline, ammonium benzoic acid, dialkoxybenzene sulfonic acid, dialkoxybenzoic acid, pyridine, pyridine monosulfonic acid, pyridine disulfonic acid, pyridine carboxylic acid and pyridine dicarboxylic acid can be co- condensated into the melamine-formaldehyde-sulfonate condensates.
  • the sulfonated ketone-formaldehyde are products in which as ketone component a mono- or diketone is used.
  • acetone, butanone, pentanone, hexanone or cyclohexanone are built into the polymer.
  • condensates are known and for example described in WO 2009/103579.
  • sulfonated acetone-formaldehyde-condensates comprise typically units of the formula (according to J. Plank et al., J. Appl. Poly. Sci.2009, 2018 – 2024): wherein m and n are typically an integer from 10 to 250, M is an alkali metall ion, for example Na + , and the ratio of m:n is generally in the region from about 3:1 to about 1:3, in particular from about 1,2:1 to about 1:1,2.
  • acetone-formaldehyde-condensates are products, which are marketed by the company BASF Construction Solutions GmbH under the trade name Melcret ® K1L.
  • aromatic building units like gallic acid, aminobenzene sulfonic acid, sulfanilic acid, phenol sulfonic acid, aniline, ammonium benzoic acid, dialkoxybenzene sulfonic acid, dialkoxybenzoic acid, pyridine, pyridine monosulfonic acid, pyridine disulfonic acid, pyridine carboxylic acid and pyridine dicarboxylic acid can be co-condensated.
  • BNS ⁇ -naphthaline-formaldehyde-condensates
  • ⁇ -naphthaline-formaldehyde-condensates are the products marketed byhe company BASF Construction Additives GmbH under the trade name Melcret ® 500 L.
  • aromatic building units like gallic acid, aminobenzene sulfonic acid, sulfanilic acid, phenol sulfonic acid, aniline, ammonium benzoic acid, dialkoxybenzene sulfonic acid, dialkoxybenzoic acid, pyridine, pyridine monosulfonic acid, pyridine disulfonic acid, pyridine carboxylic acid and pyridine dicarboxylic acid can be co-condensated.
  • the present invention relates in a second aspect to the use of the dispersion composition according to the first aspect (including all preferred embodiments) formproving flexibilisation or for providing waterproofness of particularly membranes.
  • the present invention relates in a third aspect to the use of an additive mixture (AM-a) comprising i) a polyol having the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, -OH, C 1 -C 5 -alkyl, wherein o is an integer from 0-5, and/or ii) NR 1 R 2 R 3 , wherein R 1 is C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, (CH 2 O) n
  • the cement-based sealing slurry comprises a polymer dispersion.
  • the cement-based sealing slurry comprises a Portland cement.
  • the additive mixture (AM-a) comprises components i) to iii).
  • the carbonate source is comprised in the additive mixture (AM-a).
  • the additive mixture comprising i) a polyol having the structure R 5 -(CHOH) o -R 4 , wherein R 4 and R 5 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, -OH, C 1 -C 5 -alkyl, wherein o is an integer from 0-5, and/or ii) NR 1 R 2 R 3 , wherein R 1 is C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C 1 -C 6 -aminoalkyl, (CH 2 O) n -OH, (CH 2 CH 2 O) n -OH, or (CH 2 CH 2 CH 2 O) n -OH; R 2 and R 3 are independently C 1 -C 6 -hydroxyalkyl, C 2 -C 6 -hydroxyalkenyl, C
  • the additive mixture comprises components i) to iv).
  • the additive mixture comprises i) the polyol in an amount of 5 to 30 wt.-%, ii) the NR 1 R 2 R 3 in an amount of 2 to 25 wt.-%, iii) the polycondensate or a sulfite addition product in an amount of 1 to 30 wt.-%, iv) the carbonate source in an amount of 4 to 45 wt.-%, and v) the salt of in an amount of 0 to 15 wt.-%, each based on the total weight of the additive mixture.
  • the additive mixture comprises i) the polyol in an amount of 10 to 30 wt.-%, ii) the NR 1 R 2 R 3 in an amount of 5 to 20 wt.-%, iii) the polycondensate or a sulfite addition product in an amount of 10 to 30 wt.-%, iv) the carbonate source in an amount of 25 to 45 wt.-%, and v) the salt of in an amount of 2 to 15 wt.-%, each based on the total weight of the additive mixture.
  • the additive mixture (AM-a) comprises i) the polyol in an amount of 25 to 35 wt.-%, ii) the NR 1 R 2 R 3 in an amount of 10 to 25 wt.-%, iii) the polycondensate or a sulfite addition product in an amount of 20 to 35 wt.-%, and v) the salt of in an amount of 5 to 18 wt.-%, each based on the total weight of the additive mixture (AM-a).
  • the additive mixture comprises i) the polyol in an amount of 5 to 27 wt.-%, ii) the NR 1 R 2 R 3 in an amount of 3 to 15 wt.-%, iii) the polycondensate or a sulfite addition product in an amount of 1 to 8 wt.-%, iv) the carbonate source in an amount of 4 to 17 wt.-%, and water in an amount of 50 to 80 wt.-%, each based on the total weight of the additive mixture.
  • the additive mixture (AM-a) comprises i) the polyol in an amount of 5 to 27 wt.-%, ii) the NR 1 R 2 R 3 in an amount of 3 to 15 wt.-%, iii) the polycondensate or a sulfite addition product in an amount of 1 to 8 wt.-%, and water in an amount of 55 to 80 wt.-%, each based on the total weight of the additive mixture (AM-a).
  • the use of the additive mixture and of the additive mixture (AM-a) together with a carbonate source according to the present invention provides a pot life of the cement-based sealing slurry of 0.3 to 3 hours, more preferably of 0.4 to 2.5 hours, even more preferably of 0.5 to 2 hours, and in particular of 1 to 2 hours.
  • the pot life is the use period within which the polymer-modified building material in the made-up state has a viscosity and creaminess appropriate for processing, such that it can be applied to the application substrate with a suitable aid (brick trowel, squeegee, etc.). If this period is exceeded, the building material can no longer be spread smoothly on the application substrate.
  • the pot life according to the present invention is determined via a thin film of the material to be tested having a height of from 1.5 to 3.5 mm, a width of from 10.0 to 14.0 cm, and a length of from 15 to 30 cm on a Teflon foil.
  • the use of the additive mixture and of the additive mixture (AM-a) together with a carbonate source provides a drying time of less than 4 hours, preferably of less than 3.5 hours, even more preferably of less than 3 hours, and in particular of less than 2 hours.
  • the drying of the film is preferably evaluated by applying a pressure of approximately 10 to 20 g on the film, to check when the film can no longer be plastically deformed.
  • the present invention relates in a fourth aspect to a flexible water-proofing membrane obtained from a dispersion composition according to the first aspect.
  • the preferred embodiments of the components of the dispersion composition the same preferred embodiments as for the first aspect apply.
  • the present invention relates in a fifth aspect to a method of sealing a concrete or masonry structure comprising applying to the concrete or masonry structure the dispersion composition according to the first aspect.
  • the term "concrete" denotes a mortar to which are added coarse granulates, i.e.
  • cement paste denotes the inorganic binder composition admixed with water.
  • the aggregate in this invention can be for example silica, quartz, sand, crushed marble, glass spheres, granite, limestone, sandstone, calcite, marble, serpentine, travertine, dolomite, feldspar, gneiss, alluvial sands, any other durable aggregate, and mixtures thereof.
  • the aggregates are often also called fillers and in particular do not work as a binder.
  • the dispersion composition is applied on the concrete or masonry structure in a thickness from 0.5 mm to 5 mm, more preferably from 0.8 mm to 3 mm. It is to be understood that the thickness is measured directly after the application of the dispersion on the concrete or masonry structure, i.e. in wet condition.
  • the dispersion may be applied once or multiple times.
  • the same preferred embodiments as for the first aspect apply.
  • the present invention is further illustrated by the following examples. Examples Starting materials For the examples and comparative examples, the following starting materials were used: Polymer dispersions Aqueous dispersions; Dispersion 1: In a 4 L glass vessel equipped with anchor stirrer, heating and cooling devices, and various feeds, 400.0 g of deionized water and 6.8 g of a polystyrene seed latex dispersion (with a solids content of 33% by weight; with a weight-average particle diameter of 28 nm) were heated to an internal temperature of 90 °C while stirring (140 rpm).
  • the polymer dispersion obtained had a solids content of 54.0% by weight, a number-average particle diameter of 250 nm and a glass transition temperature of -15°C.
  • Additives Polymer 1 Urea-glyoxylic acid condensate The urea-glyoxylic acid condensate was synthesized according to WO2019/077050A1: Synthetic procedure A, retarder 7 in table 1, page 24-26.
  • the resulting suspension can be used directly or can be dried to a powder which is obtainable, e.g. by drum-drying, spray drying, or flash-drying.
  • Accelerator powder 1 In a rotating drum 179.6 g spray dried urea-glyoxylic-acid condensate, 59.9 g sodium gluconate, 365.3 g sodium bicarbonate, and 110.7 g silica were filled. While the drum rotates, a mixture from 94.8 g triethanolamine (TEA) and 189.7 g glycerol were sprayed into the drum.
  • TSA triethanolamine
  • Accelerator solution 1 2.868 g of an aqueous polymer 1 solution (s.c.52.3%), 6.157 Na 2 CO 3 , 5.575 g glycerol, 2.787 g TEA, and 30.812 g water were stirred, resulting in a suspension with a solids content of 33.23%.
  • Accelerator solution 2 2.868 g of a 52.3% aqueous Polymer 1 solution, 3.079 g Na 2 CO 3 , 7.168 g glycerol, 3.584 g TEA, and 37.580 g water were stirred, resulting in a suspension with a solids content of 28.25%.
  • Accelerator solution 3 2.868 g of a 52.3% aqueous Polymer 1 solution, 3.079 g Na2CO3, 7.168 g glycerol, and 17.190 g water were stirred, resulting in a suspension with a solids content of 38.76%.
  • Accelerator solution 4 2.868 g of a 52.3% aqueous Polymer 1 solution, 7.168 g glycerol, 3.584 g TEA, and 10.3 g water were stirred, resulting in a suspension with a solids content of 39.76%.
  • Example 1 For a two-component application, 750 g of the dry compound from Table 1 was mixed with 7 g of powder 1 and 14 g CaSO 4 (anhydrite). Afterwards, 468.3 g of the dispersion 1 and 36 g water were added to the dry compound and stirred.
  • the resulting dispersion-modified mineral building material mixture has a polymer dispersion / cement ratio (p/c) of 1.09 and a water / cement ratio (w/c) of 1.08.
  • Example 2 For a two-component application, 750 g of the dry compound from table 1 was mixed with 14 g CaSO 4 (anhydrite). Separately, 468.3 g of the dispersion 1 were mixed with 41.5 g of accelerator solution 1. Afterwards, the resulting dispersion was added to the dry compound and stirred. Additional water was added until the resulting dispersion-modified mineral building material mixture has a polymer dispersion / cement ratio (p/c) of 1.09 and a water / cement ratio (w/c) of 1.08.
  • Example 3 For a two-component application, 750 g of the dry compound from table 1 was mixed with 14 g CaSO 4 (anhydrite). Separately, 468.3 g of the dispersion 1 were mixed with 48.8 g of accelerator solution 2. Afterwards, the resulting dispersion was added to the dry compound and stirred. Additional water was added until the resulting dispersion-modified mineral building material mixture has a polymer dispersion / cement ratio (p/c) of 1.09 and a water / cement ratio (w/c) of 1.08.
  • p/c polymer dispersion / cement ratio
  • w/c water / cement ratio
  • Example 4 For a one-component application where only water has to be added before usage, 750 g of the dry compound from table 1 was mixed with 7 g of powder 1, 14 g CaSO 4 (anhydrite), and 300 g RDP 1. Afterwards, water was added to the dry compound until the resulting dispersion- modified mineral building material mixture has a polymer dispersion / cement ratio (p/c) of 1.09 and a water / cement ratio (w/c) of 1.08.
  • Example 5 For a two-component application, 750 g of the dry compound from table 1 was mixed with 14 g CaSO 4 (anhydrite). Separately, 468.3 g of the dispersion 1 were mixed with 26.8 g of accelerator solution 3.
  • Comparative example 2 For a one-component application where only water has to be added before usage, 750 g of the dry compound from table 1 was mixed with 300 g RDP 1. Afterwards, water was added to the dry compound until the resulting dispersion-modified mineral building material mixture has a polymer dispersion / cement ratio (p/c) of 1.09 and a water / cement ratio (w/c) of 1.08. Comparative Example 3: For a two-component application, 750 g of the dry compound from table 1 was mixed with 14 g CaSO 4 (anhydrite). Separately, 468.3 g of the dispersion 1 were mixed with 28.8 g of accelerator solution 4. Afterwards, the resulting dispersion was added to the dry compound and stirred.
  • CaSO 4 anhydrite
  • Table 2 Cumulated heat of hydration, drying time, and pot life of the dispersion-modified mineral building material mixtures.
  • the calorimetry measurements were performed at 20°C.
  • the pot life of the above-described dispersion-modified mineral building material mixture was assessed.
  • the pot life is the use period within which the polymer-modified building material in the made-up state has a viscosity and creaminess appropriate for processing, such that it can be applied to the application substrate with a suitable aid (brick trowel, squeegee, etc.). If this period is exceeded, the building material can no longer be spread smoothly on the application substrate.
  • a pot life of 0.5-2 h is desirable, whereas faster systems are difficult to process and extremely slow systems (pot life >3 h) delay the next working steps.
  • the effect is summarized in Table 2.
  • the dispersion-modified mineral building material mixture was used to produce a wet thin film (height: 2.5 mm, width 12.0 cm and length 20 to 25 cm) on a Teflon foil.
  • the appearance of the dried building material was examined. All films were homogeneous (no separation), apparently smooth, and had no cracks.
  • the drying of the film was evaluated. For this purpose, a pressure of approximately 10-20 g was exerted by placing a finger on the film, to check when the film could no longer be plastically deformed. A short drying time ⁇ 3 h is desirable so that the next work steps are not delayed. These steps could be adding another layer of the film, applying tile adhesive, etc.
  • Table 2 the pot lives of comparative examples 3 and 4 are not sufficient.
EP22735306.7A 2021-05-27 2022-05-25 Dispersionszusammensetzung mit einer dichtungsaufschlämmung auf zementbasis und einer additivmischung Pending EP4347529A1 (de)

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