US20170183260A1 - Concrete colourants - Google Patents

Concrete colourants Download PDF

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Publication number
US20170183260A1
US20170183260A1 US15/313,821 US201515313821A US2017183260A1 US 20170183260 A1 US20170183260 A1 US 20170183260A1 US 201515313821 A US201515313821 A US 201515313821A US 2017183260 A1 US2017183260 A1 US 2017183260A1
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Prior art keywords
formulation
polycarboxylic acid
ethylene glycol
poly
cementitious
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Abandoned
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US15/313,821
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English (en)
Inventor
Rachel D'Arcy Lacy
Cameron James Tristram
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.)
Drikolor Inc
Original Assignee
D'ARCY POLYCHROME Ltd
Drikolor Inc
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Application filed by D'ARCY POLYCHROME Ltd, Drikolor Inc filed Critical D'ARCY POLYCHROME Ltd
Assigned to D'ARCY POLYCHROME LIMITED reassignment D'ARCY POLYCHROME LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LACY, Rachel D'Arcy, TRISTRAM, Cameron James
Assigned to DRIKOLOR INC reassignment DRIKOLOR INC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DPL HOLDINGS LIMITED
Publication of US20170183260A1 publication Critical patent/US20170183260A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/30—Oxides other than silica
    • C04B14/308—Iron oxide
    • C—CHEMISTRY; METALLURGY
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/022—Carbon
    • C—CHEMISTRY; METALLURGY
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/30—Oxides other than silica
    • 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
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/30—Oxides other than silica
    • C04B14/305—Titanium oxide, e.g. titanates
    • C—CHEMISTRY; METALLURGY
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/30—Oxides other than silica
    • C04B14/307—Chromium oxide
    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators or shrinkage compensating agents
    • C04B22/06—Oxides, Hydroxides
    • C—CHEMISTRY; METALLURGY
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C—CHEMISTRY; METALLURGY
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/02—Alcohols; Phenols; Ethers
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/122—Hydroxy amines
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    • 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
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
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    • 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
    • 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
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    • 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
    • C04B28/08—Slag cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/34—Compounds of chromium
    • C09C1/346—Chromium oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C—CHEMISTRY; METALLURGY
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C—CHEMISTRY; METALLURGY
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
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    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/54—Pigments; Dyes
    • C—CHEMISTRY; METALLURGY
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/80—Optical properties, e.g. transparency or reflexibility
    • C04B2111/82—Coloured materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

Definitions

  • the invention relates to methods of colouring cementitious building materials, such as concrete, and formulations for use in these methods.
  • the invention relates to a method of colouring concrete used in floor levelling and repair.
  • Cementitious building materials such as concrete are used in large volumes throughout the world. By varying the proportions of ingredients used in the cementitious premix, many types of concrete are available. These include floor levelling and repair products. Such products are used, for example, in preparing a floor prior to the laying of a covering such as carpet or vinyl. These products are designed to find their own levels when installed at a thickness of 3 mm or greater. Once hydrated and poured the cementitious mix hardens and sets rapidly so that it can be walked on within as little as two to three hours. It is often desired to improve the aesthetic qualities of building materials by introducing colour. To achieve this the surface of the building material may be either dyed or colour added during the forming of the material (referred to here as “integral colouring”).
  • a first method involves washing the surface with an acidic solution containing a metal salt. Following development of the colour a neutralising agent, then a clear protective polymeric sealing coating are applied.
  • a second method involves washing the surface with an acidic solution to roughen or etch the surface before colouring the surface with a polymer based stain or paint and finishing with a clear coating.
  • a third method involves etching or grinding the surface before applying a cementitious overlay. The cementitious overlay is then stained with an acidic solution containing a metal salt.
  • the integral colouring of concrete has been achieved by adding formulations of inorganic pigments such as iron oxide to the hydrated premix.
  • inorganic pigments such as iron oxide
  • a range of earth tones are thereby obtainable.
  • Ingredients used in the cementitious premix such as those added to provide integral colour or the requisite “self-levelling” properties of floor levelling and repair products, must not adversely affect the durability and strength of the building material once formed.
  • ingredients added to a cementitious premix to provide colour should not interfere with the function of additives included, for example, to provide “self-levelling” properties.
  • inorganic pigments such as iron oxide can inhibit the performance of shrinkage-compensating additives used in floor levelling and repair products resulting in cracking.
  • Many different formulations of pigments have been proposed for integral colouring of cementitious building materials, especially concrete.
  • colouring materials deposited on iron oxide particles obtained by precipitation include carbon black, azo colouring materials, vat dyes (anthraquinoid and indigoid) and phthalocyanine colouring materials.
  • the pigments thereby provided are proposed for use in colouring concrete, tile and brick.
  • the publication of Bowen (1980) states that it is difficult to obtain a sufficiently thorough mixing of powders into a wet cement mix so as to achieve a homogenous colour throughout the mixture.
  • the publication discloses stabilized thixotropic slurries for colouring concrete comprising pigment, at least one stabilizer, a dispersant and water.
  • the publication of Krockert and Linde (1993) discloses a process for colouring building materials.
  • the process uses inorganic pigments (iron oxides, titanium oxide) formulated as granules.
  • the granules are prepared by spray-drying aqueous suspensions of 38 to 55% by weight of the inorganic pigments and 0.3 to 1.3% by weight of soluble salts.
  • the granules are asserted to have at least satisfactory flow behaviour and rapid dispersibility in concrete.
  • the publication of Kohler et al discloses a process for the preparation of iron oxide black pigment granules which are stable to handling.
  • the process includes a step of tempering spray-dried granules of iron oxide black pigment in an indirectly heated rotary kiln at temperatures below 65° C. in an inert nitrogen atmosphere for approximately 30 to 60 minutes.
  • the granules are asserted to have high strength, dispersibility and stability to oxidation.
  • the publication of Will (1998) discusses how many inorganic pigments, such as metal oxides, do not disperse well in cementitious systems.
  • the publication discloses a method for colouring cementitious systems using compacted inorganic granules.
  • the compacted inorganic granules comprise an inorganic pigment and a dispersing agent.
  • Johansen et al (1999) discloses an aqueous composition for colouring cement-based composition comprising water, pigment, a suspension enhancing agent and latex polymer solids.
  • a mixture of predetermined amounts of a cement-based component and the aqueous composition is asserted to provide a cement-based composition of uniform and standardised colour that is capable of being consistently reproduced.
  • compositions for colouring concrete discloses a composition for colouring concrete.
  • the composition includes a stearic acid, salt or derivative as a hydrophobic efflorescence control agent.
  • the composition also includes particulated polymers and co-polymers. The composition is asserted to improve durability of the coloured concrete.
  • the publication of Noack and Herrmann (2004) discloses colouring pigment granulates.
  • the granulates comprise granulated cores that do not contain binders, emulsifying agents, surface active agents, dispersing agents, or preservatives.
  • the granulates cores are enclosed by an enveloping layer made of a material such as polyvinyl alcohol, that can be broken down.
  • the absence of binders and other auxiliaries is asserted to ensure rapid disagglomeration once the shell enveloping material is broken down.
  • compositions for colouring concrete when integrally or surface-shake applied discloses compositions for colouring concrete when integrally or surface-shake applied.
  • the composition comprises a spray-dried styrene acrylic polymer encapsulated colourant and a second polymer for use in dispersing the encapsulated colourant.
  • the standard of Anon (2010) prescribes that coloured concrete pigmented at a maximum dosage rate of 10% by weight of the cement shall have a 28-day compressive strength of not less than 90% and a water to cement ratio of not greater than 110% of that of the control.
  • the standard further prescribes that when added to concrete at the maximum dosage rate, the pigment is to neither accelerate the initial or final set by more than one hour nor retard the initial or final set by more than one and a half hours, and the air content is not be changed by more than 1% as compared to the control.
  • the invention provides a flowable, spray dried, particulate formulation suitable for use in colouring cementitious building materials comprising in admixture one or more inorganic pigments, poly(ethylene glycol), hydroxylated amine and polycarboxylic acid.
  • the one or more pigments of the formulation are inorganic pigments selected from the group consisting of: synthetic iron oxides (black, browns, red and yellows); natural iron oxides; chromium oxide; cobalt blue; cobalt green; titanium dioxide and carbon black (concrete grade).
  • the first aspect of the invention provides a flowable, spray dried, particulate formulation consisting essentially of one or more inorganic pigments, poly(ethylene glycol), hydroxylated amine and polycarboxylic acid in admixture.
  • the formulation comprises poly(ethylene glycol), polycarboxylic acid dispersant and hydroxylated amine in a 2-6:2-6:1 ratio by weight. More preferably, the formulation comprises poly(ethylene glycol), polycarboxylic acid dispersant and hydroxylated amine in a 2-4:4-6:1 ratio by weight. Most preferably, the formulation comprises in admixture poly(ethylene glycol), polycarboxylic acid dispersant and hydroxylated amine in a 3:5:1 ratio by weight.
  • the poly(ethylene glycol) has a median molecular weight in the range 7,000 to 9,000 (PEG 8000).
  • the hydroxylated amine is 2-amino-2-methyl-1-propanol.
  • a preferred 2-amino-2-methyl-1-propanol is supplied under the trade name AMP 95TM (CAS#124-68-5).
  • the polycarboxylic acid dispersant is a carboxylated acrylic co-polymer.
  • a preferred acrylic acid polymer is supplied under the trade name RHODOLINE 226/40TM (CAS# 9003-04-7).
  • the polycarboxylic acid is less than 5% by weight of the formulation.
  • the formulation consists essentially of the one or more inorganic pigments, the poly(ethylene glycol), the polycarboxylic acid dispersant and the hydroxylated amine in a 45-160:2-6:2-6:1 ratio by weight. More preferably, the formulation consists essentially of the one or more pigments, the poly(ethylene glycol), the polycarboxylic acid dispersant and the hydroxylated amine in a 45-125:2-6:2-6:1 ratio by weight. Yet more preferably, the formulation consists essentially of the one or more pigments, the poly(ethylene glycol), the polycarboxylic acid dispersant and the hydroxylated amine in a 45-110:2-6:2-6:1 ratio by weight. Most preferably, the formulation consists essentially of the one or more pigments, the poly(ethylene glycol), the polycarboxylic acid dispersant and the hydroxylated amine in a 45-110:3:5:1 ratio by weight.
  • the particles of the formulation are of a hollow doughnut morphology with a median diameter in the range 20 to 150 ⁇ m. More preferably, the particles of the formulation are of a hollow doughnut morphology with a median diameter of 30 to 50 ⁇ m.
  • the invention provides a colourant product that is a flowable, spray-dried, particulate formulation consisting essentially of 85 to 95% by weight of one or more inorganic pigments, 3 to 7% by weight of poly(ethylene glycol) having a median molecular weight in the range 7,000 to 9,000 (PEG 8000), 3 to 6% by weight carboxylated acrylic co-polymer dispersant and 0.5 to 2.0% by weight hydroxylated amine.
  • a colourant product that is a flowable, spray-dried, particulate formulation consisting essentially of 85 to 95% by weight of one or more inorganic pigments, 3 to 7% by weight of poly(ethylene glycol) having a median molecular weight in the range 7,000 to 9,000 (PEG 8000), 3 to 6% by weight carboxylated acrylic co-polymer dispersant and 0.5 to 2.0% by weight hydroxylated amine.
  • the invention provides a method of colouring a cementitious building material comprising the step of mixing a formulation of the first aspect of the invention with a cementitious premix.
  • the cementitious premix is hydrated immediately prior to the step of mixing the formulation with the cementitious premix. More preferably, the cementitious premix is a floor levelling or repair product.
  • the cementitious building material is selected from the group consisting of: concrete, mortar and plaster.
  • the invention provides an integrally coloured cementitious building material comprising one or more pigments, poly(ethylene glycol), polycarboxylic acid and hydroxylated amine.
  • the cementitious building material is selected from the group consisting of: concrete, mortar and plaster. More preferably, the building material is concrete. Most preferably, the building material is a levelled or repaired concrete floor.
  • admixture means an intimate, uniform mixture of two or more components
  • building material means a hardened cementitious material including concrete, mortar and plaster
  • cement means reducing, oxidising or desiccating by roasting or strong heat
  • cement means a powdery substance made by calcining lime and clay used in making mortar and concrete
  • cementitious building material means a building material prepared by mixing cement and water with or without the addition of aggregate or sand
  • cementitious premix means a mixture of cement and water used in the forming of a building material such as concrete, mortar or plaster
  • colourant means a formulation including primary particles of one or more pigments used in preparing a coloured base medium such as a cementitious building material
  • colouring means dispersing one or more pigments uniformly throughout a building material and “coloured” has a corresponding meaning
  • comprising means “including”, “containing” or “
  • the presence, concentration or a ratio of ingredients is specified the presence, concentration or ratio specified is the initial presence, concentration.
  • values are expressed to one or more decimal places standard rounding applies. For example, 1.7 encompasses the range 1.650 recurring to 1.7499 recurring.
  • FIG. 1 Heat output curves for mortars prepared using cement sourced from Golden Bay (plots 2 and 4 ) or Holcim (plots 1 and 3 ) with (plots 1 and 2 ) or without (plots 3 and 4 ) the addition of 2% (w/w) of a superplasticiser (CD31).
  • a superplasticiser CD31
  • FIG. 2 Schematic representation of a single-point discharge configuration of a spray dryer ( 1 ) of the type used in the methods described provided with an inlet ( 2 ), an outlet ( 3 ) and a rotary atomiser ( 4 ).
  • FIG. 3 Heat output curves for coloured mortars prepared using unformulated pigments and corresponding formulations prepared according to the invention. Heat output curves are shown overlain on the heat output curve for unadulterated cement (Control). All mortars were prepared using cement sourced from Golden Bay.
  • FIG. 4 Heat output curves for coloured mortars prepared using unformulated pigments and corresponding formulations. Heat output curves are shown overlain on the heat output curve for unadulterated cement (Control). All mortars were prepared using cement sourced from Holcim.
  • FIG. 5 Heat output curves for coloured mortars prepared using unformulated pigments and corresponding formulations prepared according to the invention. Heat output curves are shown overlain on the heat output curve for unadulterated cement (Control), All mortars were prepared using cement sourced from Dricon.
  • FIG. 6 Photographs of samples of the hardened cementitious floor levelling product SIKATM LEVEL 30 (Sika (NZ) Limited) with (A) and without (B) the addition of colourant.
  • the hydration of cementitious premixes by the addition of water initiates ettringite formation.
  • This primary ettringite formation is important in the hardening and setting of concrete and is to be distinguished from the delayed ettringite formation associated with damage to hardened concrete.
  • the shape and size of the ettringite crystals is influenced by the composition of the alkaline solution in which the crystals are forming.
  • the hardening and setting of concrete can be monitored by calorimetric methods.
  • cementitious premixes formulated for use as rapid setting floor levelling and repair products are designed to find their own levels when installed at a thickness of 3 mm or greater. Once hydrated and poured the cementitious mix hardens and sets rapidly so that it can be walked on within as little as two to three hours.
  • the cementitious premixes used in floor levelling and repair are formulated with specially selected polymers to provide these performance characteristics.
  • the invention resides partly in the selection of a combination of formulants that do not have a significant deleterious effect on the hardening and setting of cementitious building materials when mixed with a hydrated cementitious premix.
  • the invention also resides partly in this combination of formulants being compatible with the spray drying of aqueous formulations of the inorganic pigments used in colouring cementitious building materials.
  • the invention permits the formulation of a range of these pigments as flowable granules of uniform density that may be dispensed gravimetrically or volumetrically, thereby facilitating the use of these pigments in colouring cementitious building materials.
  • the invention will be illustrated with reference to the use of the combination of a poly(ethylene glycol), a polycarboxylic acid and a hydroxylated amine in the preparation of flowable, spray dried, particulate formulations of inorganic pigments that readily disperse when added to hydrated cementitious premixes.
  • the use of this combination of formulants does not adversely affect the primary ettringite formation as evidenced by no observed deleterious effects on the hardening and setting of the building material.
  • the flowable, spray dried, particulate formulations are prepared by dispersing the pigments in an aqueous solution of the formulants. Dispersions of different pigments may be blended if desired prior to spray drying.
  • a schematic representation of single-point discharge configuration of a spray dryer fitted with a rotary atomiser is provided in FIG. 2 .
  • a solution of poly(ethylene glycol) 8,000 g/mol (PEG 8000) in water was prepared at a ratio of 10% (w/w) by dissolving 90 g of the PEG 8000 in 900 g of water with gentle agitation.
  • the solution was then blended with 150 g of a polycarboxylic acid dispersant (RHODOLINE 226/40) and 30 g of a hydroxylated amine (AMP 95).
  • 3,000 g of green oxide pigment was slowly added with continuous stirring up to 3,000 rpm for a total of 80 minutes to provide a homogenous dispersion.
  • the homogenous dispersion was then spray-dried using a GEA Niro MOBILE MINORTM (GEA Process Engineering) equipped with a rotary atomiser (channel wheel, 20,000 rpm) in a single-point discharge configuration and operated at an inlet temperature of 185° C. and outlet temperature of 95° C.
  • a particulate formulation of hollow doughnut morphology with a median particle diameter of 30 ⁇ m was obtained at a rate of 1.9 Kg/hour (1.2% w/w moisture content) with 52% yield.
  • a selection of poly(ethylene glycol) 8,000 g/mol (PEG 8000) in water was prepared at a ratio of 6% (w/w) by dissolving 75 g of the PEG 8000 in 1250 g of water with gentle agitation.
  • the solution was then blended with 125 g of a polycarboxylic acid dispersant (RHODOLINETM 226/40) and 25 g of a hydroxylated amine (AMP 95).
  • RHODOLINETM 226/40 polycarboxylic acid dispersant
  • AMP 95 a hydroxylated amine
  • 2,500 g of red ochre pigment was slowly added to provide a raw homogenous dispersion.
  • the raw homogenous dispersion was then ball-milled for a total of 12 hours to provide a final milled homogenous dispersion.
  • the homogenous dispersion was then spray-dried using a GEA Niro MOBILE MINORTM (GEA Process Engineering) equipped with a rotary atomiser (channel wheel, 20,000 rpm) in a single-point discharge configuration and operated at an inlet temperature of 185° C. and outlet temperature of 95° C.
  • a particulate formulation of hollow doughnut morphology with a median particle diameter of 30 ⁇ m was obtained at a rate of 1.9 Kg/hour (1.2% w/w moisture content) with 52% yield.
  • Examples 3 to 6 Similar quantities of colourants (Examples 3 to 6) were prepared by methods similar to those employed for the preparation of the colourants of Example 1 and Example 2. Larger quantities of colourants (Examples 7 to 9) were prepared using a GEA Niro VERSATILE-SDTM 6.3N (GEA Process Engineering).
  • Example 7 The colourant of Example 7 was spray-dried with an inlet temperature of 230° C. and an outlet temperature of 85° C. at a production rate of 23 Kg/h with a pressure nozzle configuration and final moisture content of less than 1.5%.
  • Example 8 The colourant of Example 8 was spray-dried with an inlet temperature of 230° C. and an outlet temperature of 95° C. at a production rate of 55 Kg/h with a pressure nozzle configuration and final moisture content of less than 1.5%.
  • Example 9 The colourant of Example 9 was spray-dried with an inlet temperature of 220° C. and an outlet temperature of 90° C. at a production rate of 60 Kg/h with a pressure nozzle configuration and final moisture content of less than 1.5%.
  • Quantity Ingredient (with 111.6 Kg water) (Kg) Ratio Iron oxide red (Red 5530)(Nubolia) (CAS# 1309-37-1) 450.3 100 Poly(ethylene glycol) (PEG 8000) 13.5 3 Polycarboxylic acid dispersant (RHODOLINE 226/40) 20.1 4.5 Hydroxylated amine (AMP 95) 4.5 1
  • compositions of a series of spray-dried colourants comprising chrome green oxide as the pigment.
  • Ingredient G1 G2 G3 G4 G5 G6 G7 Poly(ethylene glycol) 6 6 6 6 6 6 3 14.4 (PEG 8000) Polycarboxylic acid dispersant 1.4 3.6 5 7.5 5 5 6 (RHODOLINE TM 226/40) Hydroxylated amine 1 1 1 1 5 1 1.2 (AMP 95)
  • the quantities of the ingredients are expressed as a percentage by weight of the pigment.
  • Each one of the spray-dried colourants from the series was evaluated by mixing at a rate of 2% (w/w) with a slurry of cementitious building material consisting of 225 g water, 500 g dry sand and 1,000 g ordinary Portland cement.
  • the formulation was spray-dried using the Mini Spray Dryer B-290 (Buchi) with an inlet temperature of 180° C. and an outlet temperature of 105° C.
  • the product of spray-drying would not disperse when added to an aqueous slurry of concrete. This was attributed to a surface layer of sodium silicate not hydrating rapidly enough to release the primary particles of pigment.
  • the formulation was spray-dried using the GEA Niro MOBILE MINORTM with an inlet temperature of 180° C., an out let temperature of 95° C. and a spindle speed of 15,000 rpm.
  • the product of spray-drying was mixed at a rate of 3% (w/w) with a slurry of cement (1:2 (w/w) water-cement) comprising no aggregate. Hydration of the cementitious mix was found to be indefinitely retarded.
  • the formulation was spray-dried using the Mini Spray Dryer B-290 (Buchi) with an inlet temperature of 180° C. and an outlet temperature of 105° C.
  • the product of spray-drying was mixed at a rate of 4% (w/w) with a slurry of cement (1:2 (w/w) water-cement).
  • Example 3 The colourants of Example 3, Example 4, Example 5 and Example 6 were evaluated for use in colouring concrete or mortar prepared using cement from three different sources (Golden Bay, Holcim and Dricon). The colourants were evaluated against their corresponding unformulated pigments (milled iron oxides) with (Example 4, Example 5 and Example 6) or without (Example 3) the addition of fumed silica. The colourants were evaluated for any adverse effects on the setting and hardening characteristics of the resulting cementitious building material calorimetry was used to evaluate early age hydration of the cementitious building material. Compressive strengths of 50 mm cubes of cement mortar was determined at 48 hours, 7 days and 28 days.
  • FIG. 3 Golden Bay
  • FIG. 4 Holcim
  • FIG. 5 Density plots for coloured mortars prepared using the different sources of cement are presented in FIG. 3 (Golden Bay), FIG. 4 (Holcim) and FIG. 5 (Dricon).
  • the absence of any significant variation between the heat flows measured confirms the compatibility between the colourants with the cementitious building material.
  • FIG. 1 the effect on heat flows of the addition of a commonly used plasticizer (2% by weight of DC31) is shown in FIG. 1 .
  • Colourants were added at a rate of 3% by weight to a slurry of cement (0.4 (w/w) water-cement) and the compressive strength of hardened blocks (50 ⁇ 50 ⁇ 50 mm) determined. Slurries were prepared using cement sourced from either Golden Bay or Holcim. The compressive strength determined for coloured hardened blocks prepared using these two sources of cement are presented in Table 2 (Golden Bay) and Table 3 (Dricon). Compressive strengths were also determined for coloured hardened blocks prepared by the addition of colourant at a rate of 3% by weight to a slurry of cement and sand (0.4 (w/w) water-cement and 1.5 (w/w) sand-cement). The compressive strengths determined for the coloured hardened blocks are presented in Table 4 (Golden Bay) and Table 5 (Dricon). The moderate reduction in strength (circa 10%) may be readily compensated for by addition of cement to the premix.

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  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
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MY132071A (en) * 1995-05-11 2007-09-28 Cure Corp C A composition and method for dispersing pigment in cement based compositions
DE19704943A1 (de) * 1997-02-10 1998-08-13 Bayer Ag Anorganische Pigmentgranulate zum Einfärben von Kunststoffen, Lacken und Baustoffen und ein Verfahren zu deren Herstellung
DE19706899C1 (de) * 1997-02-21 1998-11-05 Bayer Ag Anorganische, kompaktierte Pigmentgranulate, Verfahren zu ihrer Herstellung und ihre Verwendung
CA2263667C (fr) 1999-03-15 2002-02-26 Axel J. Societe En Commandite Procedes de fabrication de granules de pigments et de coloration de beton
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US9382158B2 (en) 2016-07-05
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US20150336849A1 (en) 2015-11-26

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