WO2001074735A1 - Procede de production de granules pigmentaires et de coloration des betons - Google Patents

Procede de production de granules pigmentaires et de coloration des betons Download PDF

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Publication number
WO2001074735A1
WO2001074735A1 PCT/CA2000/000346 CA0000346W WO0174735A1 WO 2001074735 A1 WO2001074735 A1 WO 2001074735A1 CA 0000346 W CA0000346 W CA 0000346W WO 0174735 A1 WO0174735 A1 WO 0174735A1
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WO
WIPO (PCT)
Prior art keywords
pigment
drying
mixture
binder
producing
Prior art date
Application number
PCT/CA2000/000346
Other languages
English (en)
Inventor
Daniel Fortin
Marie-Paule Jacoulet
Axel E. Jungk
Mark Roberts
Original Assignee
Axel J. Societe En Commandite
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
Priority to CA002263667A priority Critical patent/CA2263667C/fr
Application filed by Axel J. Societe En Commandite filed Critical Axel J. Societe En Commandite
Priority to PCT/CA2000/000346 priority patent/WO2001074735A1/fr
Priority to AU2000235473A priority patent/AU2000235473A1/en
Publication of WO2001074735A1 publication Critical patent/WO2001074735A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/02—Agglomerated materials, e.g. artificial aggregates
    • C04B18/022—Agglomerated materials, e.g. artificial aggregates agglomerated by an organic binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006—Preparation of organic pigments
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0092—Dyes in solid form
    • 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
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

Definitions

  • the present invention relates to a process for producing pigment granules and to the granules obtained therefrom.
  • the present invention also relates to a process for dyeing concrete and other materials with the granules obtained by the process according to the invention.
  • granules means agglomerates and aggregates of materials with an average diameter ranging from 30 ⁇ m to 2 mm, initially in a powder state, and/or in the state of a suspension and/or of a solution.
  • pigments relates to organic and/or inorganic dyes, including white pigments as example such as titanium dioxide, the various red, yellow, brown and black iron oxides and their mixtures, carbon blacks, chromium oxide, manganese oxide and/or cobalt spinelles and others.
  • crete relates to the raw material which contains among other things, before any chemical reacting: cement or other hydraulic binders, and/or fly ashes, silicates, sands and/or aggregates and other components, for example for producing plates, tiles, paving stones, interlocking paving stones, parpens, and for the realization of concrete binding for example.
  • cement or other hydraulic binders and/or fly ashes, silicates, sands and/or aggregates and other components, for example for producing plates, tiles, paving stones, interlocking paving stones, parpens, and for the realization of concrete binding for example.
  • cement also covers mortar or cement, fibre-cement compounds and other articles initially containing cement and/or hydraulic binders.
  • Concrete is a well-proven material in construction, which in its form of decorative concrete, also satisfies aesthetic requirements.
  • the dyeing of the concrete mass for producing decorative concrete provides the latter with a long- lasting tint, requiring nearly no maintenance for years.
  • concrete surfaces, decorated by the application of a paint coating need to be repainted at short intervals.
  • Colored concrete is used for example for facades, plates, cobblestones, tiles, anti-noise embankments, retaining walls, dikes, bridges and similar constructions, and in the form of colored mortar and of roughcast, also for decorating facades.
  • Concrete is colored by inorganic pigments and more recently by organic pigments.
  • organic pigments For example, manganese oxide, iron oxide, chromium oxide, and carbon have proved to be suitable pigments for concrete application. More particularly, pigments made of carbon, and iron oxide, appeared to be very efficient in practice.
  • the producing of colored concrete nevertheless gives rise to the following problems.
  • the powder of pigments produces dust and its use soils humans, machines and premises.
  • the pastes cannot be stocked for very long in the silos or in other greatly dimensioned containers since they separate by segregation of the components and result partially in solid deposits.
  • briquettes have dominated in the field of coal and minerals.
  • micro-capsules are used for carbon paper.
  • the fodder is stocked in silos, in the form of compact granules.
  • lacquers concentrates of pigments in nitrocellulose are used, free of dust which are dissolved perfectly in solvents.
  • carbon black is used in the form of granules obtained by aggregation.
  • PCV is used in the form of pearled granules obtained by atomisation and by drying of its aqueous suspensions.
  • Patent No. FR-A-2,450,273 describes pearled granules containing pigments made of dry carbon, but at the same time, with a water content of 59%, with little dust. These granules are used for dyeing cement.
  • EP-A-0, 268,645 and its equivalents in the United States (US-A-4,946,505) and in Canada (CA-A-1 ,291 ,849) describe the coloring of concrete with the help of pigment granules, except for compacted or "briquetted" granules, which are made of one or more pigments, pure carbon pigments being excluded, and obligatorily, with the help of one or more binders, which promote the dispersing of the pigments in the concrete.
  • the specific binders described in this document are well defined. In comparison to concretes colored with pure pigments and without additives, they can generate an increase of the efflorescence in concrete.
  • pigments in the form of granules exhibit an insufficient dispersion, lack tinting strength and, in order to reach the same result, need to be applied in a higher amount than powder,
  • pigments in the form of granules which contain a binder do not show improved dispersing effects
  • the humidity present in the concrete is not sufficient for dissolving granules which contain a binder.
  • the granules of pigment obtained according to this complicated process present no advantage when compared to the granules obtained by the process according to the patent No. US-A-4,496,505.
  • European patent No. EP-B-0, 802,241 of the Bayer AG company describes a granulation process, similar to the above mentioned compacting process, for the carbon black pigment, with the same drawbacks.
  • European patent No. EP-B-0,697,379 describes, in general terms, the formation of granules in a "fluid bed dryer".
  • the patent No. EP-A-0,657,511 describes a particular form of the patent No. US-4,496,505 by using as binders sugars which belong to the family of polyhydroxy substances described in the patent No. US-A-4,495,505 even though the sugars used are known to modify the properties of concretes in a negative way.
  • EP-A-0,58,152 uses soluble salts as binders for granules and as an agent which promotes the dispersion of pigments in the concrete. But, since these granules are also not mechanically stable, they still bring a lot of dust and they are not free flowing.
  • European patent No. EP-A-0,507,046 describes granules for coloring concrete with the "advantage" of a supplementary agglomeration step of the granules, once that these granules have been prepared according to the spray granulation process. Moreover, this process does not bring satisfying results regarding the free flowing of these granules, the absence of dust and the simplicity of the process. In fact, it is a more complicated version of the process described in the patent No. EP-A-0,482,450 which uses certain salts as binders in a process of granulation by agglomeration, without a spray granulation step being required.
  • European patent No. EP-B-0,482,449 describes granules of inorganic pigments, which contain impurities already present in the pigments from their production process, i.e. the inorganic salts.
  • This patent claims any process for dyeing concrete with granules, already described in the prior art and containing pigments (iron oxide).
  • the granules according to this patent exhibit the same drawbacks as the granules of the preceding patent with respect to the problems related to the dust and to the lack of free flow.
  • EP-B-0,395,872 describes granules of black iron oxide, made by spray granulation of an aqueous suspension of this oxide with an unstable organic substance, which in practice works like a dispersing agent for the preparation of the aqueous suspension with a high content in pigments (50-75%), as already described in the patent No. US-A-4,946,505; after granulation the dispersant is destroyed by an additional thermal process, which has to be applied after the spray granulation at very high temperatures.
  • the three main objects of the present invention are:
  • the granules according to the invention are free of dust, free flowing, non hygroscopic and do not form agglomerates due to the presence of humidity. Moreover, these new granules, despite the prejudices mentioned in lines 23 to 52, column 2 of the patent No. US-A-4,946,505, disperse well in concrete with the same tinting strength as that of the granules of the patent No. US-A-4,946,505, as that of the corresponding pigments in form of powder and are well dispersed in the medium to be dyed. Moreover, the granules according to the invention exhibit an additional advantage when compared to those containing dispersants, in the sense that they do not negatively influence the mechanical elimination of water in wet concretes.
  • the granules according to the invention are, except for impurities, free of dispersants and/or surfactants or of other chemical compounds soluble in water, as it is the case, among other things, for those granules described in the patent No. US-A-4,495,505, which contain binders allowing promotion of the dispersion of granules into concrete.
  • the granules according to the invention are free of dispersing binders that are soluble in water, they avoid the promotion of efflorescence in concrete and the formation of hard balls, during their storage under the influence of humidity, balls insoluble in concrete.
  • the insoluble and inactive binders contained in the granules according to the invention neither exhibit the negative effects generated by the additives of the prior art upon the hardening of the concrete.
  • the first object of the present invention is reached by the process for producing pigment granules comprising the following steps of:
  • the second object of the present invention is reached by a process for dyeing concrete using as dyes granular pigments obtained by the process according to the first object of the invention as dyes.
  • pigment granules comprising:
  • binders selected from the group consisting of organic compounds which form insoluble films after drying and/or by chemical reaction accompanying the drying, said binders being chosen such that the films thereby obtained are free of dispersing effects in concrete,
  • the percentages being weight percentages expressed with respect to the total weight of pigment granules.
  • the pigment granules according to the invention contain less than 4% of water and from 81 to 99.95% of pigments.
  • a mixture in the form of a liquid suspension, of an emulsion and/or of a paste is prepared, said mixture comprising at least one pigment and at least one organic binder of a specific nature.
  • the mixture eventually contains one or more additives for concretes.
  • the liquid used for the preparation of the mixture is water.
  • the binders used in the preparation of the mixture are: organic compounds which form insoluble films after drying and/or by chemical reaction accompanying the drying, and more particularly
  • each binder being selected such that the films thereby obtained are free of dispersing effects in concrete.
  • the mixture additionally contains chemical additives which react with the binder during the drying of said mixture.
  • binders which by drying and/or by chemical reaction and/or by the presence of reactive additives, become insoluble and form a film, stabilising the mechanical properties of the granules without affecting their coloring effect,
  • said binders being further selected such that the films thereby obtained are free of dispersing effects in concretes.
  • the binder used is selected from the group consisting of the polyacrylates, the copolymers of styrene and polyacrylic acids, the vinyl acrylates, the copolymers of styrene and of acrylates, the copolymers of maleic acid anhydride, and the latex used in paints such as those described in the following table:
  • the binders are present in the form of a suspension or an aqueous emulsion.
  • resins or other chemical compounds are used as binders which form insoluble films in water during the drying by reacting with reactive additives.
  • binders are used, that display a well developed dispersing capability. This allows to obtain mixtures made of liquid, preferably water, of pigments, of binders with a dispersing effect and of other additives with a very high volumetric concentration of pigments; these binders are used with reactive additives that by chemical reaction with one or more binders, particularly by reticulation, become insoluble in water and weather resistant and form films and stabilise the mechanical properties of granules without disturbing the coloring power.
  • the binder is selected from the group consisting of resins and systems of resins used for preparing varnishes and/or paints.
  • the binders with a high dispersing capacity particularly well adapted for the formation of water insoluble films by a reticulation reaction with reactive additives, and free of dispersing effect in concrete, are polymer acids in their acid forms, the polymer acids in their partially neutralized form and the polymer acids in their neutralized form. More particularly, they are polycarboxylic and polyacrylate acids. As an example of polymer acids and polycarboxylic acids, the Carbopol * and the BF-Goodrich "K * -700 Series" in a partially neutralised state.
  • polyacrylates in their acidic or partially neutralized form such as the Rhom and Haas Acrysol* G-111 , or such as some polyacrylates sold by Allied Colloids, BASF.
  • the amount of binder present in the granules varies between 0.05 to 15% in weight with respect to the total weight of granules, preferably between 0.5 to 8% in weight and more particularly between 0.8 and 5% in weight.
  • the mixture contains in weight from 0.1 to 15% of binder with respect to the weight of pigments present in the mixture.
  • each binder exhibits before drying, plasticizing and/or tensioactive effects and these properties are not present anymore after drying.
  • catalysts are used with the binders i.e. substances which, during the step of drying leading to granulation, are completely evaporated and potentially recuperated by cooling of vapours and recycled.
  • These volatile catalysts have as a function to facilitate the dispersion of pigments in the liquid mixture and to reach a higher volumetric concentration of pigments in said mixture. This is important for the diameter of the obtainable granules, particularly during a drying granulation by atomisation, but also for the amount of liquid which is evaporated, in order to obtain a certain amount of granules, which is then reduced.
  • the amount of catalyst present in the mixture ranges from 0.1 to 15% in weight with respect to the weight of pigment present in the mixture.
  • These volatile catalysts allow to sensibly increase the amount of pigment in the mixtures containing pigments, binders and other additives.
  • AMP is of particular interest as a volatile catalyst.
  • the volatile catalyst is recovered during the drying step and recycled into the process.
  • the volatile catalyst is recovered by cooling.
  • the chemical reactive additives which can also exhibit dispersing effects, and which react with said binders by forming insoluble films in water by reticulation during and/or by the drying step and which allow, to sensibly increase the amount of pigment in the mixtures comprising the pigments, binders and additives are, for example, polyols such as polyethylene glycols (Macol BASF)
  • 1 ,8-dihydroxyantraquinone, of anthrarufin, of 3,5 dihydroxybenzoic acid, of 1 ,5-dihydroxynaphtalene, of 3-hydroxy-2,2-dimethylpropyl 3-hydroxy- 2,2-dimethylpropionate of acetylenes such as Surfinol * 104, Surfinol * 104 PG50, Surfinol* 104 DPM, Surfinol * 104 E, Surfinol*104 BC, Surfinol* 400 Series (Air Products), glycol silicone (BASF Corp.), sugars and modified polyurethane such as EFKA* 452 of LUBRIZOL.
  • the reactive chemical additives are used in an amount ranging from 0.1 to 15% with respect to the weight of pigments present in the mixture.
  • pH regulators are sodium acetate, carbonates, NaOH, ammonium salts and sulphuric acids.
  • the mixture containing preferably water, binders, optionally dispersive volatile catalysts and/or reactive chemical additives, and pigments may contain one or more additives useful for concrete.
  • Pigment granules obtained according to one of the processes of the invention are used for coloring concrete or other materials. They contain among other things, water, the above mentioned pigments, binders in the form of their films insoluble in water and, eventually, other additives useful for concrete.
  • the amount of volatile catalyst introduced in the mixture but missing in the granules ranges from 0 to 15% in weight with respect to the weight of a granule.
  • the amount of reactive additives and of reticulants introduced in the mixture before drying represents from 0 to 15% in weight of a granule.
  • the pigments used for preparing the mixture are of organic and/or inorganic nature.
  • inorganic pigments are preferably selected, pigments from the group of the manganese oxides, iron oxides and hydroxides, chromium oxides, titanium dioxides, carbon blacks and spinelles, particularly cobalt spinelles. It is also possible to use exclusively organic, exclusively inorganic and mixtures of organic and inorganic pigments.
  • Well suited for the process of dyeing concrete according to the invention are fine granules, with a size between 30 ⁇ and 3 mm, preferably between 35 ⁇ and 2 mm, more particularly between 40 and 500 micrometers and particularly suited are granules of a size between 40 ⁇ and 400 ⁇ obtained by drying and granulation of a mixture containing:
  • phase preferably water
  • the pigment granules obtained contain:
  • binders selected from the group consisting of the organic compounds which form insoluble films after drying and/or by chemical reaction accompanying the drying, the percentages being weight percentages expressed with respect to the total weight of the granule.
  • the pigment granules preferably contain less than 4% of water and from 79 to 99.95% of pigments.
  • binders selected from the group consisting of the organic compounds which form insoluble films after drying and/or by chemical reaction accompanying the drying;
  • the percentages being weight percentages expressed with respect to the total weight of the granule.
  • the pigment granules obtained are preferably in the form of pearls.
  • the mixtures of pigment granules obtained by one of the processes of the invention contain at least 90% of pearls with a size ranging from 40 to 400 microns.
  • the state of the art there is a multitude of different ways to produce pigment granules from mixtures in the form of a liquid suspension, of an emulsion and/or of a paste.
  • the granules according to the invention may be obtained in different ways by drying a mixture of binders, pigments, liquid, preferably water, eventually volatile catalysts and/or reactive additives and, if needed, of other additives.
  • Another way to proceed consists in preparing the mixture and to extrude it with the help of an extruder according to the so called “spaghetti” or “angel hairs” process which is commonly used in the pasta food industry, then by drying it with warm air or by contact with a warm surface and by grinding the strings of
  • Yet another way to produce granules according to the invention consists in applying very small drops of this mixture on a heated surface and to separate these small dried drops from the surface.
  • the preferred form for the granules according to the invention is the pearled granule.
  • Said pearled granules are obtained from mixtures of the liquids described above by an atomizer dryer via pipes having one or several nozzles at their end or respectively spray disks placed in a spray tower.
  • the pearled granules are in the form of micro granules; 90% of the pigment particles have a size ranging from 20 to 500 ⁇ , particularly a size ranging from 40 to 400 ⁇ .
  • the granules produced and used according to the invention flow freely from a silo and do not tend to agglomerate nor to form agglomerates. They are easily transported by pneumatic means. At the same time, they have a lower sensibility to humidity and show less tendency for forming agglomerations or hard balls, than the granules containing water soluble dispersants or even hygroscopic dispersants as binders.
  • the handling of granules according to the invention produces practically no dust. From a handling point of view, the granules are superior to those of the prior art. Thus, producing and use of the granules according to the invention are therefore particularly suited for a clean and automatic dyeing, more particularly of concrete. Due to these facts, they are of excellent use in practice.
  • the product obtained was a pearled granule and 98% of the pearls had a size ranging from 45 ⁇ to 375 ⁇ .
  • Those granules were free flowing, were free of dust and had a residual humidity ranging from 0.3 to 1.3%.
  • the bulk density ranged from 0.81 to 1.04 g/l.
  • the pearled granules thus obtained had an average size ranging from 150 to 200 ⁇ and exhibited a good mechanical stability.
  • aqueous suspension composed of: 0.9% of binder which is a copolymer of polyacrylic with styrene, 1.13% of amino methyl propanol as volatile catalyst, 60% of red iron oxide and of water for the rest, pearled granules were prepared in the same way as described in Example 1.
  • the inlet temperature of the drying air ranged from 280° to 340°C; the outlet temperature of the air was between 110° and 170°C.
  • the granules obtained were raw, 78% of them had a size ranging from 355 ⁇ to 45 ⁇ , they were free flowing and were dust free. Their residual humidity ranged from 0.3 to 0.1% and the bulk density ranged from 0.800 to 1.100 g/l.
  • aqueous suspension composed of: 0.9% of binder, a copolymer of polyacrylic acid with styrene, 1.13% of amino methyl propanol as a volatile catalyst, 40% of yellow iron oxide and water for the remaining part, pearled granules were prepared in the same way as described in Example 1.
  • the inlet temperature of the drying air ranged from 280° to 340°C, the outlet temperature of the air ranged from 110° to 170°C.
  • the obtained granules were raw, 78% of the grains had a size ranging from 355 ⁇ to 45 ⁇ , were free flowing and were dust free. Their residual humidity ranged from 0.3 to 2.9% and the bulk density ranged from 500 to 1.100 g/l.
  • Example 4 The same procedure as described in Example 4 was used. Instead of pearled granules obtained according to the invention, the same amount of black iron oxide (10.4 kg) in the form of granules with a binder which promotes the dispersing of pigments in concrete, i.e. of Granufin Onyx * of the Davis society, was used.
  • Example 4 red pearled granules according to Example 2 in an amount of 11.3 kg were used.
  • Example 5 Then the shades of the humid concretes obtained as in Example 5 were compared with those obtained as in Example 5a, and thereafter the shades of pavements dried for 24 hours.
  • Example 5 For coloring, 11.3 kg of pigments in a powder form used for producing granules according to Example 2 was used.
  • Example 5 It is proceeded as described in Example 5.
  • 11.3 kg of yellow pearled granules according to Example 3 were used.
  • Example 6 A comparison was made between the shades of the humid concretes obtained as in Example 6 with those obtained in Example 6a, and thereafter the shades of the pavements dried for 24 hours. Neither in the humid concrete, nor in the dried concrete, could differences of colors be seen.
  • Example 5 For coloring, 11.3 kg of yellow powder pigments were used, the same powder used to produce granules according to Example 3.
  • Example 6 The shades of the humid concretes obtained in Example 6 were compared with those obtained in Example 6b, and thereafter the shades of pavements dried for 24 hours. Neither in the humid concrete, neither in the dried concrete, could differences of color be seen.
  • An aqueous mixture of 150.00 ml of water, of 10.00 g of K-702 * as a reticulating binder, of 2.19 g of propylene glycol as reactive additive and of 2.20 g of AMP-95 as a volatile catalyst was prepared; then 2.00 g of NH 4 HCO 3 was added in order to obtain a pH of 8, and then 303 g of red pigment (Hematite) was added.
  • this mixture was put in the form of small drops on a glass plate and dried at 110°C. After drying, small drops with a diameter of about 1 mm were obtained. 10 g of those pearls were put into water for 72 hours; they did not decompose.
  • the whole was further mixed for 2 minutes, then the mortar obtained was poured into a 3 cm deep square form.
  • the form was conserved at ambient temperature for 24 hours.
  • the mortar obtained was poured into a 3 cm deep square form.
  • the form was conserved for 24 hours at ambient temperature. Then the body of the mortar was extracted from the form.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)

Abstract

L'invention concerne un procédé de production de granulés pigmentaires comprenant les étapes suivantes : a) préparation d'une mixture, se présentant sous la forme d'une suspension liquide, d'une émulsion et/ou d'une pâte, ladite mixture comprenant au moins un pigment et au moins un liant sélectionné dans le groupe constitué par les composants organiques qui forment des pellicules insolubles après séchage et/ou par réaction chimique pendant le séchage, chaque liant étant sélectionné de sorte que les pellicules ainsi obtenues n'aient pas d'effet dispersant dans les bétons ; et b) séchage de ladite mixture. Les granulés obtenus résistent à l'humidité et sont utilisés pour la coloration de bétons.
PCT/CA2000/000346 1999-03-15 2000-03-30 Procede de production de granules pigmentaires et de coloration des betons WO2001074735A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CA002263667A CA2263667C (fr) 1999-03-15 1999-03-15 Procedes de fabrication de granules de pigments et de coloration de beton
PCT/CA2000/000346 WO2001074735A1 (fr) 1999-03-15 2000-03-30 Procede de production de granules pigmentaires et de coloration des betons
AU2000235473A AU2000235473A1 (en) 1999-03-15 2000-03-30 Process for producing pigment granules and for dyeing concrete

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA002263667A CA2263667C (fr) 1999-03-15 1999-03-15 Procedes de fabrication de granules de pigments et de coloration de beton
PCT/CA2000/000346 WO2001074735A1 (fr) 1999-03-15 2000-03-30 Procede de production de granules pigmentaires et de coloration des betons

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WO2001074735A1 true WO2001074735A1 (fr) 2001-10-11

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DE102009019846A1 (de) * 2009-05-06 2010-11-11 H.C. Carbon Gmbh Granulatzusammensetzung und Verfahren zu deren Herstellung
US8461229B2 (en) 2006-10-25 2013-06-11 Basf Se Heat-stable encapsulated pigments
US9120950B1 (en) 2014-03-05 2015-09-01 D'arcy Polychrome Limited Pigment formulations
WO2015178784A1 (fr) * 2014-05-23 2015-11-26 Lacy Rachel D Arcy Colorants de béton

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AU2002952194A0 (en) 2002-10-22 2002-11-07 Silica Pacific Pty. Limited Composition and method for colouring the surface of a porous substrate

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EP0365046A1 (fr) * 1986-06-09 1990-04-25 Chemische Werke Brockhues Ag Procédé pour la coloration du béton
US4946505A (en) * 1986-06-09 1990-08-07 Chemische Werke Brockhues Ag Process for dyeing concrete
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Cited By (12)

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Publication number Priority date Publication date Assignee Title
US7365109B2 (en) * 2000-09-15 2008-04-29 Merck Patent Gmbh Pigment preparation in granulate form
US8461229B2 (en) 2006-10-25 2013-06-11 Basf Se Heat-stable encapsulated pigments
DE102009019846A1 (de) * 2009-05-06 2010-11-11 H.C. Carbon Gmbh Granulatzusammensetzung und Verfahren zu deren Herstellung
US9120950B1 (en) 2014-03-05 2015-09-01 D'arcy Polychrome Limited Pigment formulations
WO2015133912A1 (fr) * 2014-03-05 2015-09-11 D'arcy Polychrome Limited Préparations de pigments faciles à disperser et leur utilisation dans la coloration de milieux de base
US9441130B2 (en) 2014-03-05 2016-09-13 Drikolor Inc Easily dispersible formulations of pigments and their use in tinting base media
US9441137B2 (en) 2014-03-05 2016-09-13 Drikolor Inc Easily dispersible formulations of pigments and their use in tinting base media
WO2015178784A1 (fr) * 2014-05-23 2015-11-26 Lacy Rachel D Arcy Colorants de béton
US9382158B2 (en) 2014-05-23 2016-07-05 Drikolor Inc Method of preparing a coloured self-levelling cementitious floor covering
AU2015202815B2 (en) * 2014-05-23 2016-07-07 Drikolor Inc Concrete colourants
CN107108354A (zh) * 2014-05-23 2017-08-29 德瑞科拉公司 混凝土着色剂
AU2015262102B2 (en) * 2014-05-23 2019-04-04 Drikolor Inc Concrete colourants

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AU2000235473A1 (en) 2001-10-15
CA2263667C (fr) 2002-02-26

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