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
  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
  • C04B35/62625—Wet mixtures
  • C04B35/62635—Mixing details
• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
  • C04B20/10—Coating or impregnating
  • C04B20/1055—Coating or impregnating with inorganic materials
  • C04B20/1059—Pigments or precursors thereof
• • 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
  • C04B33/00—Clay-wares
  • C04B33/02—Preparing or treating the raw materials individually or as batches
  • C04B33/13—Compounding ingredients
  • C04B33/14—Colouring matters
• • 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
  • C04B33/00—Clay-wares
  • C04B33/36—Reinforced clay-wares
• • 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
  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
  • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
• • 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
  • C09C1/0009—Pigments for ceramics
• • 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
  • C09C1/28—Compounds of silicon
  • C09C1/30—Silicic acid
  • C09C1/3045—Treatment with inorganic compounds
  • C09C1/3054—Coating
• • 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
  • C01P2006/12—Surface area
• • 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
  • C01P2006/19—Oil-absorption capacity, e.g. DBP values
• • 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
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
  • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
• • 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
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
• • 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
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/52—Constituents or additives characterised by their shapes
  • C04B2235/528—Spheres
• • 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
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/54—Particle size related information
  • C04B2235/5409—Particle size related information expressed by specific surface values
• • 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
  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/54—Particle size related information
  • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
  • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
  • Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]

Definitions

• the present invention relates to the use of precipitated silica, having a high absorption capacity, as a raw material for obtaining a dye by impregnating said silica with an inorganic pigment in the form of a soluble salt, in particular with an inorganic pigment based on soluble iron sulfate.
• It also relates to a dye capable of being obtained by calcination, then optional grinding, of a precipitated silica having a high absorption capacity, previously impregnated with an inorganic pigment in the form of soluble salt, in particular of an inorganic pigment based on soluble iron sulfate.
• Natural or synthetic pigments are used as colorants in the ceramic industry, in particular for the production of traditional colored tiles and tiles.
• the coloring is carried out by the addition of specific pigments to the ceramic paste before the shaping by pressing and sintering of the tiles / tiles obtained.
• the Thiviers sandstone generally comprising approximately 90% of quartz and approximately 10% of goethite (FeOOH), makes it possible to obtain colors from red to brown which are the main colors developed traditionally for tiles and especially floor tiles. , and in particular porcelain stoneware tiles (Grès Porcellenato) obtained using a “fast firing” process.
• a new concept of dye for ceramic materials has recently appeared: it consists in previously including the pigment in a mineral matrix, more particularly silica.
• the potential advantage of including the pigment in an inert glassy or crystallized matrix is the great stability with respect to severe thermal and chemical conditions, such as those encountered in the ceramic industry, and has thus made it possible the development of new coloring powders.
• this dye acts as a chromatic unit from a pigmentation point of view and the color is not developed by introduction of an ion into the lattice of the matrix or by formation of a solid solution; the crystals responsible for coloring are in fact small crystals included during the cooking / sintering process of the matrix.
• a red / brown dye prepared by mixing an iron pigment, a powdered matrix based on silica and auxiliary additives such as a silicone oil, said mixing being carried out rather in the dry state; the dye is here obtained directly sa, ns the need to implement a calcination step.
• a dye made from microsilica (or silica fume) and iron oxide is described in WO 00/53680: the process uses intensive grinding in a humid environment, drying, high temperature calcination and grinding.
• the mixture between silica and iron oxide must be perfect. This implies for example that the silica powder is extremely well disaggregated by intensive grinding in order to obtain agglomerates having a size close to or less than that of the iron pigment, that is to say a few microns.
• the intensive contact of silica with the pigment is of great importance in the formation of color, in particular for obtaining a high level of red, a high gloss and a high intensity (red / brown after cooking). This is particularly the case in the presence of intensive grinding of the constituents.
• One of the aims of the present invention is to provide an alternative to the techniques known from the prior art, while dispensing with an intense grinding step and while making it possible, in particular, to achieve very good colorimetric performance. (in particular high stability), and avoiding the drawbacks mentioned above.
• the invention firstly relates to the use of precipitated silica with a high absorption capacity, preferably in the form of particles of average size of at least 50 ⁇ m, as a raw material for the obtaining a dye by impregnating said silica (therefore in solid form) with an inorganic pigment in the form of a soluble salt in solution.
• Said inorganic pigment is preferably based on a metallic compound (for example a soluble metallic salt), and, even more preferably, based on an iron compound.
• This iron compound is generally soluble iron sulfate (iron sulfate solution), soluble iron nitrate (iron nitrate solution) or a mixture thereof.
• the precipitated silica used in the context of the invention has a high absorption capacity.
• Said precipitated silica preferably has a DOP oil uptake of at least 260 ml / 100 g, in particular at least 300 ml / 100 g.
• the DOP oil intake is determined according to standard NFT 30-022 (March 1953) by using dioctylphthalate.
• Said silica can be in the form of substantially spherical beads, the average size of which is preferably as indicated above.
• the term “precipitated silica” is understood to mean a silica obtained by the precipitation reaction of a silicate, such as an alkali metal silicate (sodium silicate for example), with an acid (sulfuric acid for example); the mode of precipitation of the silica can be arbitrary here: in particular, addition of acid on a silicate base stock, simultaneous total or partial addition of acid and silicate on a base stock of water or silicate solution .
• the drying of the cake obtained by filtration of the suspension resulting from the precipitation is here preferably carried out using an atomizer, in particular a turbine atomizer, or, in particular when it is desired to use a silica present under in the form of substantially spherical beads, a nozzle atomizer, at liquid pressure or with two fluids.
• the drying can be preceded by a fluidification operation (disintegration) of the cake.
• the fluidification operation makes it possible in particular to lower, if necessary, the viscosity of the cake to be dried.
• the precipitated silica used according to the invention can be prepared for example according to preparation methods as described in EP 0520862, WO 99/07237, WO 99/49850.
• the precipitated silica used according to the invention can also be a precipitated silica such as the Tixosil 38A silica sold by the Applicant.
• the precipitated silica used in the context of the invention preferably has a BET specific surface of at least 50 m 2 / g, in particular at least 75 m 2 / g, in particular at least 90 m 2 / g, for example between 100 and 400 m 2 / g. It can be between 100 and 250 m 2 / g, in particular between 110 and 250 m 2 / g.
• the BET specific surface is determined according to the BRUNAUER - EMMET - TELLER method described in "The Journal of the American Chemical Society", Vol. 60, page 309, February 1938 and corresponding to standard NF T 45007 (November 1987).
• inorganic pigment in general, 2 to 30%, in particular 5 to 25%, for example 5 to 15%, by weight of inorganic pigment relative to the weight of silica + pigment can be used.
• Precipitated silica (advantageously amorphous) with high absorption capacity, preferably in the form of particles of average size of at least 50 ⁇ m, can be easily impregnated with the inorganic pigment in the form of an (aqueous) solution of soluble salt without no grinding is not necessary.
• a mixer of the Patterson type so-called “pants” mixer
• Kenwood, Eirich, Lôdige an internal mixer of the Brabender type.
• the impregnated silica obtained is preferably subjected to calcination, optionally after prior drying.
• An addition of silica (in solid form) can be carried out.
• the calcination is generally carried out at a temperature between 600 and 1300 ° C, in particular between 700 and 1300 ° C, preferably between 800 and 1200 ° C.
• the calcination can thus be carried out at a temperature between 800 and 1000 ° C, or, at a higher temperature, in this case between 1000 and 1200 ° C, depending on the colorimetric parameters sought in the final ceramic material after firing.
• the duration of the calcination is preferably at least 30 minutes, in particular at least 45 minutes, for example between 45 and 80 minutes.
• the calcination can advantageously be carried out at a temperature of between 1000 and 1200 ° C., for at least 45 minutes, for example for 45 to 80 minutes.
• a fine dye powder is thus obtained, for example having a BET specific surface area between 10 and 75 m 2 / g, in particular between 15 and 75 m 2 / g, for example between 15 and 50 m 2 / g; it can be between 20 and 50 m 2 / g, in particular between 20 and 40 m 2 / g.
• the subject of the invention is also a dye (capable of being) obtained by calcination, then optional grinding, of a precipitated silica with high absorption capacity, preferably in the form of particles of average size of at least 50 ⁇ m, previously impregnated with an inorganic pigment in the form of a soluble salt in solution.
• the dye according to the invention or resulting from the use, according to the invention, of a precipitated silica with high absorption capacity, preferably being in the form of particles of average size of at least 50 ⁇ m, previously impregnated using an inorganic pigment in the form of a soluble salt solution, is particularly suitable for coloring ceramic materials, for example stoneware, in particular porcelain stoneware (Porcellenato Stoneware), due to its very good colorimetric properties; it gives them, in particular in the case where the initial inorganic pigment used is based on an iron compound, in particular a high gloss and a high intensity (red / brown).
• the invention can also make it possible not to use auxiliary additives such as a silicone oil or a silane. In addition, it does not require the use of sol-gel type techniques such as for example the controlled flocculation of silica.
• the dye, in powder form, can be mixed with the ceramic paste before shaping by pressing and (after optional drying) firing / sintering at high temperature (in particular between 1000 and 1300 ° C, for example between 1200 and 1250 ° C), in particular for 20 to 150 minutes, for example between 25 and 70 minutes or between 45 and 90 minutes, of total cycle (coloring in the mass).
• high temperature in particular between 1000 and 1300 ° C, for example between 1200 and 1250 ° C
• 20 to 150 minutes for example between 25 and 70 minutes or between 45 and 90 minutes, of total cycle (coloring in the mass).
• Ceramic materials for example formed from sandstone, in particular porcelain stoneware, containing at least one dye as described above constitute one of the objects of the invention.
• These ceramic materials may in particular be tiles, tiles for example made of porcelain stoneware, in particular red to brown in color when the initial inorganic pigment used is based on an iron compound.
• the dye according to the invention or resulting from the use, according to the invention, of a precipitated silica with high absorption capacity, preferably being in the form of particles of average size of at least 50 ⁇ m, beforehand impregnated with an inorganic pigment in the form of a soluble salt in solution (aqueous), is also suitable for coloring materials with a hydraulic or bituminous binder.
• a hydraulic or bituminous binder containing at least one such dye also constitute one of the objects of the invention.
• a silica with a high absorption capacity in the form of substantially spherical beads (marketed by the Applicant) is impregnated with a solution of iron sulphate (proportions: 10% by weight of iron sulphate and 90% by weight of silica ( dry equivalent)).
• the impregnated silica obtained is dried then calcined at 1000 ° C., then ground so as to obtain a fine powder of dye.
• the dye thus prepared is introduced into a ceramic stoneware type paste (Porcellanoto Stoneware), in the following proportions: 4% by weight of dye and 96% by weight of ceramic paste. After homogenization, the composition obtained is moistened with 4% by weight of water, shaped by pressing, then, after drying, sintered at 1225 ° C for 60 minutes (total cycle).
• the colorimetric parameters of the sintered ceramic material are such that: L ⁇ 65; a> 10; 10 ⁇ b ⁇ 18.
• a silica with a high absorption capacity Tixosil 38A (precipitated silica marketed by the Applicant) is impregnated with a solution of iron sulfate II (origin: company Millenium).
• the proportions are as follows: 10% by weight of Fe 2 O 3 and 90% by weight of silica (dry equivalent) (iron content at 6.6%).
• the iron sulphate II solution is prepared by kneading for 30 minutes: 212.5 g of sulphate powder per 100 g of water. Dissolution is facilitated by heating to 55 ° C.
• the silica is then impregnated with this solution of iron sulphate in an internal mixer (Brabender type) by mixing for 25 minutes at 100 rpm.
• the proportions are as follows: 79.5 g of solution per 100 g of silica in solid form (powder).
• the product obtained is then dried at 90 ° C for 6 hours.
• the dried product is sieved to 100 microns in order to remove any possible agglomerate.
• the dye thus prepared is introduced into a ceramic paste of the sandstone type.
• the composition obtained is moistened with 4% by weight of water, then shaped by pressing in order to obtain pellets.
• the pellets are then dried at 120 ° C (for 6 hours), then introduced into a sintering oven. Sintering is carried out in a static oven at 1225 ° C - 10 minutes for a total cycle of 60 minutes.
• a silica with high absorption capacity Tixosil 38A (precipitated silica sold by the Applicant) is impregnated with a solution of iron nitrate III (origin: Prolabo company). The proportions are as follows: 10% by weight of Fe 2 0 3 and 90% by weight of silica (dry equivalent) (iron content at 6.6%).
• the iron nitrate III solution is prepared by kneading for 30 minutes: 262.5 g of nitrate powder per 100 g of water. Dissolution is carried out at room temperature (21 ° C).
• the silica is then impregnated with this iron nitrate solution in an internal mixer (Brabender type) by mixing for 25 minutes at 100 rpm.
• the proportions are as follows: 145 g of solution per 100 g of silica in solid form (powder).
• the product obtained is then dried at 90 ° C for 6 hours. The dried product is sieved to 100 microns, in order to remove any possible agglomerate.
• the dye thus prepared is introduced into a ceramic stoneware type paste (Grès Porcellenato), in the following proportions: 4% by weight of dye and 96% by weight of ceramic paste.
• the composition obtained is moistened with 4% by weight of water, then shaped by pressing in order to obtain pellets.
• the pellets are then dried at 120 ° C (for 6 hours), then introduced into a sintering oven. Sintering is carried out in a static oven at 1225 ° C - 10 minutes for a total cycle of 60 minutes.
• a silica with a high absorption capacity Tixosil 38A (precipitated silica marketed by the Applicant), is impregnated with a solution of iron sulfate II (origin: company Millenium). The proportions are as follows: 10% by weight of Fe 2 0 3 and 90% by weight of silica (dry equivalent) (iron content at 6.6%).
• the iron sulphate II solution is prepared by kneading for 30 minutes: 212.5 g of sulphate powder per 100 g of water. Dissolution is facilitated by heating to 55 ° C. The silica is then impregnated with this solution of iron sulphate in an internal mixer (Brabender type) by mixing for 25 minutes at 100 rpm.
• the product obtained is then dried at 90 ° C for 6 hours, then calcined in air. Two tests were carried out, with different calcination conditions: i) at 1020 ° C for 60 minutes; ii) at 1100 ° C for 60 minutes. After calcination, the product is roughly crushed so as to obtain a fine powder of dye: the particle size is fixed by sieving at 100 ⁇ m.
• the dye thus prepared is introduced into a ceramic stoneware type paste (Grès Porcellenato), in the following proportions: 4% by weight of dye and 96% by weight of ceramic paste.
• the composition obtained is moistened with 4% by weight of water, then shaped by pressing in order to obtain pellets.
• the pellets are then dried at 120 ° C (for 6 hours), then introduced into a sintering oven. Sintering is carried out in a static oven at 1225 ° C - 10 minutes for a total cycle of 60 minutes.
• the colorimetric parameters of the sintered ceramic material are such that:
• a silica with high absorption capacity Tixosil 38A (precipitated silica sold by the Applicant) is impregnated with a solution of nitrate of III (origin: Prolabo company). The proportions are as follows: 10% by weight of Fe 2 O 3 and 90% by weight of silica (dry equivalent) (iron content at 6.6%).
• the iron nitrate III solution is prepared by kneading for 30 minutes: 262.5 g of nitrate powder per 100 g of water. Dissolution is carried out at room temperature (21 ° C).
• the silica is then impregnated with this iron nitrate solution in an internal mixer (Brabender type) by mixing for 25 minutes at 100 rpm.
• the product obtained is then dried at 90 ° C for 6 hours, then calcined in air.
• the product After calcination, the product is roughly crushed so as to obtain a fine powder of dye: the particle size is fixed by sieving at 100 ⁇ m.
• the dye thus prepared is introduced into a ceramic stoneware type paste (Grès Porcellenato), in the following proportions: 4% by weight of dye and 96% by weight of ceramic paste.
• the composition obtained is moistened with 4% by weight of water, then shaped by pressing in order to obtain pellets.
• the pellets are then dried at 120 ° C (for 6 hours), then introduced into a sintering oven. Sintering is carried out in a static oven at 1225 ° C - 10 minutes for a total cycle of 60 minutes.
• the colorimetric parameters of the sintered ceramic material are such that:

Landscapes

• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Ceramic Engineering (AREA)
• Organic Chemistry (AREA)
• Materials Engineering (AREA)
• Structural Engineering (AREA)
• Manufacturing & Machinery (AREA)
• Dispersion Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Physics & Mathematics (AREA)
• Thermal Sciences (AREA)
• Pigments, Carbon Blacks, Or Wood Stains (AREA)

Applications Claiming Priority (3)

Publications (1)

Family

ID=27772248

Family Applications (1)

Country Status (5)

Families Citing this family (1)

Family Cites Families (9)

• 2002
  • 2002-03-12 FR FR0203478A patent/FR2837207B1/fr not_active Expired - Fee Related
• 2003
  • 2003-03-12 WO PCT/FR2003/000796 patent/WO2003076523A1/fr not_active Application Discontinuation
  • 2003-03-12 AU AU2003227826A patent/AU2003227826A1/en not_active Abandoned
  • 2003-03-12 EP EP03725280A patent/EP1483337A1/de not_active Withdrawn
  • 2003-03-12 US US10/507,238 patent/US20050166800A1/en not_active Abandoned

Non-Patent Citations (1)

Also Published As

Similar Documents

Legal Events