Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
  • C09D5/02—Emulsion paints including aerosols
  • C09D5/024—Emulsion paints including aerosols characterised by the additives
  • C09D5/028—Pigments; Filters
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
  • A23L29/03—Organic compounds
  • A23L29/035—Organic compounds containing oxygen as heteroatom
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
  • A61K33/10—Carbonates; Bicarbonates
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/44—Elemental carbon, e.g. charcoal, carbon black
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/60—Preparation of carbonates or bicarbonates in general
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F11/00—Compounds of calcium, strontium, or barium
  • C01F11/18—Carbonates
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F11/00—Compounds of calcium, strontium, or barium
  • C01F11/18—Carbonates
  • C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F11/00—Compounds of calcium, strontium, or barium
  • C01F11/18—Carbonates
  • C01F11/186—Strontium or barium carbonate
  • C01F11/187—Strontium carbonate
• • 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
  • C09C1/02—Compounds of alkaline earth metals or magnesium
  • C09C1/021—Calcium carbonates
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D11/00—Inks
  • C09D11/02—Printing inks
  • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
  • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D11/00—Inks
  • C09D11/30—Inkjet printing inks
  • C09D11/32—Inkjet printing inks characterised by colouring agents
  • C09D11/322—Pigment inks
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
  • C09D7/60—Additives non-macromolecular
  • C09D7/61—Additives non-macromolecular inorganic
• • D—TEXTILES; PAPER
  • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
  • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
  • D21H19/00—Coated paper; Coating material
  • D21H19/36—Coatings with pigments
  • D21H19/38—Coatings with pigments characterised by the pigments
  • D21H19/385—Oxides, hydroxides or carbonates
• • 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
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/01—Particle morphology depicted by an image
  • C01P2004/03—Particle morphology depicted by an image obtained by SEM
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/30—Particle morphology extending in three dimensions
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/51—Particles with a specific particle size distribution
• • 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
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 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
  • C01P2006/12—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
  • C01P2006/60—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
  • C01P2006/88—Isotope composition differing from the natural occurrence
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
  • C08K3/24—Acids; Salts thereof
  • C08K3/26—Carbonates; Bicarbonates
• • 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
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/10—Biofuels, e.g. bio-diesel
• • 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
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

Definitions

• the invention relates to a new synthetic mineral material containing carbonate whose decomposition reduces the rate of emission of carbon dioxide fossil fuel.
• this new mineral material batch cascades still said continuously or batch-continuous mixing and its uses in the various fields that are the pharmaceutical field, the field of food or feed, or the paper industry, in particular the manufacture of paper, mass or coating, or any other surface treatment of paper as well as the fields of aqueous or non-aqueous paints, as well as the field of plastics such as in particular that of polyethylene films. breathable or the field of printing inks.
• the first object of the invention is a new synthetic mineral material containing carbonate having a high level of carbon 14 ( 14 C).
• Another object of the invention is a method of manufacturing synthetic mineral materials containing carbonate having a high level of carbon 14 ( 14 C).
• a further object of the invention is the use of synthetic mineral materials according to the invention in the aforementioned fields.
• the Applicant intends mineral pigment and / or mineral filler.
• the synthetic mineral material containing carbonate having a high level of 14 C according to the invention is characterized in that it has a nuclear conversion rate of carbon of 14 C at 12 C of at least 450 transformations per hour and per gram, preferably between 700 and 890 transformations per hour and per gram, very preferably between 850 and 890 transformations per hour and per gram.
• the carbon conversion rate in carbon from 14 C to 12 C of the synthetic mineral material is carried out according to a method of determining the rate of nuclear transformation whose originality lies in the stage sample preparation.
• the conventional methods for analyzing the nuclear conversion rate in carbon from 14 C to 12 C known to date are based on a preparation step consisting of a thermal decomposition at high temperature (approximately 1000 0 C) by combustion or calcination of the sample to be analyzed and then of the collection of carbon dioxide released and trapped at a low temperature before its reduction, by catalytic hydrogenation, to an elemental carbon atom whose composition is isotope 13 C / 12 C and 15 N / 14 N and 14 C is measured by a mass spectrophotometer.
• the Applicant has developed a method for determining the rate of nuclear transformation characterized by a step of preparation of the sample by means of an H 3 O + donor, such as in particular hydrochloric acid, or of other donors of H 3 O + stronger than carbonic acid such as phosphoric acid, and which allows to dose only the carbon from the inorganic or mineral phase of the sample to be analyzed.
• This method for determining the 14 C nuclear conversion rate at 12 C of the synthetic mineral material containing the carbonate according to the invention is characterized in that it comprises: a) a step of preparing the sample consisting of an attack of the sample by an H 3 O + donor, preferably hydrochloric acid or any H 3 O + donor, stronger than carbonic acid such as 'Phosphoric acid,
• a preferred variant of the process for determining the degree of nuclear conversion is characterized in that an additional trap having a temperature of 20 ° C. is added between the acid etching step and the carbon dioxide recovery stage. ° C at 30 ° C above the trap of step b), to avoid contamination with other volatile compounds from the sample.
• the Applicant emphasizes that the nuclear conversion rates of 450 transformations per hour and per gram, preferably between 700 and 890 transformations per hour and per gram, very preferably between 850 and 890 transformations per hour and per gram, and which are the essential characteristic of the product object of the invention, may nevertheless be determined by any other appropriate method.
• the sample to be analyzed according to the invention consists of the mineral material containing carbonate according to the invention, and can be a sheet of paper containing the mineral material, a calcium carbonate treated with organic compounds, a composition of polyvinyl (PVC), a calcium carbonate having organic impurities or any other sample.
• the inorganic materials according to the invention are characterized in that the carbonate is chosen from carbonates of monovalent and / or bivalent and / or trivalent cations or their mixtures.
• these inorganic materials according to the invention are characterized in that said monovalent and / or bivalent and / or trivalent cations are chosen from the cations of the first or second main group of the periodic table of Mendeleiev.
• said cations are chosen from lithium, sodium, potassium, magnesium, calcium, strontium or their mixtures.
• the synthetic mineral material containing a carbonate according to the invention is preferably characterized in that it is a calcium carbonate having a crystalline structure of the calcite or aragonite or vaterite type or in that it is a mixture of a carbonate of calcic type structure calcium with a calcium carbonate of aragonite type structure and / or a calcium carbonate of vaterite-type structure, and more preferably in that it is a mixture of calcite-type structure and aragonite type.
• said calcium carbonate according to the invention with the aforementioned crystalline structure is characterized in that it has a degree of whiteness greater than 80%, preferably greater than 90%, very preferably greater than 93% TAPPI determined according to the TAPPI standard. T452 ISO 2470.
• the synthetic mineral material containing carbonate according to the invention is characterized in that it is a mixture and / or a co-structure of the abovementioned carbonates with other mineral materials chosen from silicas. natural and / or synthetic, silicates such as in particular clay, talc, mica, or else chosen from aluminum hydroxides, sulphates, satin whites, phosphates such as brushites, octa-calcium phosphates or hydroxyapatites, or mixtures thereof.
• the process for manufacturing the mineral materials according to the invention is characterized in that it uses carbon dioxide resulting from aerobic or anaerobic fermentation, preferably anaerobic and more particularly derived from the fermentation of sugars or the combustion of alcohol. from the fermentation of organic compounds.
• carbon dioxide resulting from aerobic or anaerobic fermentation, or the fermentation of sugars or the combustion of alcohol from the fermentation of organic compounds will be called fresh carbon dioxide.
• inverse fossil fuel carbon dioxide resulting from the combustion of fossil fuels such as coal, oil or natural gas, or carbon dioxide from the calcination of natural calcium carbonate which will be called old carbon dioxide.
• the fresh carbon dioxide is derived from the fermentation of sugars or the combustion of alcohol, in particular ethanol, methanol, or alkanes such as methane, ethane, or any other alkane, originating from the fermentation of organic compounds such as fruit, fruit alcohols or waste from landfills or is the result of fermentation or thermal decomposition or oxidative degradation of waste from supercritical pressure landfills.
• alcohol in particular ethanol, methanol, or alkanes such as methane, ethane, or any other alkane, originating from the fermentation of organic compounds such as fruit, fruit alcohols or waste from landfills or is the result of fermentation or thermal decomposition or oxidative degradation of waste from supercritical pressure landfills.
• the fresh carbon dioxide used in the process according to the invention is a mixture of fresh carbon dioxide from the fermentation of sugars with fresh carbon dioxide from the combustion of organic compounds.
• Another variant of the process according to the invention is characterized in that it implements a mixture of carbon dioxide resulting from aerobic or anaerobic fermentation, preferably anaerobic and more particularly derived from the fermentation of sugars or the combustion of alcohol. from the fermentation of organic compounds, with old carbon dioxide.
• the process according to the invention is characterized in that the mixture uses less than 50% by weight of old carbon dioxide.
• the method of manufacturing synthetic mineral material containing carbonate according to the invention is characterized in that the implementation of carbon dioxide is carried out at a temperature between 5 ° C and 100 ° C, preferably between 20 ° C. and 30 ° C.
• This process according to the invention is characterized in that it is a process in batch, in cascades still said continuous or in continuous-batch mixing.
• the Applicant hears a manufacturing process in which the reaction takes place in a single tank where all the reagents are introduced.
• the Applicant understands a manufacturing process in which the fresh carbon dioxide used is introduced into a cascade of n reactors installed in series and / or in parallel whose assembly in series is illustrated by the drawing n ° 1.
• n the number of cascaded reactors in which carbon dioxide and / or any other additive are introduced continuously, this number n ranging from 1 to 50, preferably from 1 to 10, very preferably from 1 to 5.
• the Applicant intends a continuous synthesis process followed by one or more steps in batch, this or these last steps may be the addition of carbon dioxide storage or addition of various additives or still a physical treatment step (such as grinding, centrifugation, thermal concentration, mechanical concentration) or a chemical treatment step such as treatment with sodium silicate followed by addition of an acid such as acid citric acid or phosphoric acid or optionally at least one step of introducing a dispersant.
• a physical treatment step such as grinding, centrifugation, thermal concentration, mechanical concentration
• a chemical treatment step such as treatment with sodium silicate followed by addition of an acid such as acid citric acid or phosphoric acid or optionally at least one step of introducing a dispersant.
• drawing No. 2 illustrating this batch-batch mixing process, the Applicant designates by "m" the number of physical or chemical treatment mentioned above, this or these treatments which can be in particular a treatment by mechanical concentration by implementing a centrifuge.
• This number "m” varies from 1 to 5, preferably from 1 to 2.
• the Applicant indicates by "o" the number of steps corresponding to a possible addition of dispersant, this dispersant being any type of dispersant known to those skilled in the art whose choice is adapted so obvious to those skilled in the art depending on the intended application.
• This number “o” varies from 0 to 3, preferably from 0 to 1.
• the method according to the invention is finally characterized in that it optionally comprises at least one dispersion step and / or at least one step of grinding in a dry medium or in a humid medium, in the presence of optionally at least one dispersing agent and / or at least one grinding aid agent.
• the inorganic materials according to the invention are used in the pharmaceutical field with products such as drugs, the field of food or feed, or the paper industry such as papermaking, mass and / or coating on a paper or plastic medium or any other surface treatment of paper and / or plastic, the plastic being preferably chosen from polyolefins of the polyethylene or polypropylene type and their derivatives, as well as the fields of aqueous paints or non-aqueous as well as the field of plastics or the field of printing inks.
• the use of mineral materials in the coating of paper is preferably done during blade coating operations, film transfer, water curtain or by "size-press".
• the use of inorganic materials as paper mass filler is preferably done by adding the mineral material according to the invention to different locations before and / or during the formation of the sheet.
• the inorganic materials according to the invention used in the field of printing inks are used in inks for inkjet printing, offset printing and / or rotogravure printing.
• This example illustrates various processes of the prior art using an old carbon dioxide.
• This test which illustrates the prior art, relates to a process for producing calcium carbonate precipitated by reacting lime with old carbon dioxide from the combustion of fossil energy such as butane.
• This test which illustrates the prior art, relates to a process for producing calcium carbonate precipitated by reacting lime with old carbon dioxide from the calcination of natural calcium carbonate.
• old carbon dioxide gas from calcination is reacted in a muffle furnace at 900 ° C. with a ground natural calcium carbonate ( Omyapure TM from Omya SAS), with a suspension of lime at 10% by weight of dry matter.
• a ground natural calcium carbonate Omyapure TM from Omya SAS
• the product obtained which is a precipitated calcium carbonate of the prior art, is then dried at 140 ° C.
• This test which illustrates the prior art, relates to a process for producing strontium carbonate by reaction of strontium hydroxide with old carbon dioxide from the calcination of natural calcium carbonate.
• the Sr (OH) 2 x 8 (H 2 O) strontium hydroxide (Lot 9329 A from Riedel-de Ha ⁇ n) is suspended in a container containing water without carbon dioxide for forming a suspension of strontium hydroxide at a solids concentration of 10% by weight.
• old carbon dioxide obtained from calcination in a muffle furnace at 900 ° C. of a ground natural calcium carbonate (Omyapure TM), is introduced at ambient temperature (22 ° C. ⁇ 20 ° C.). from Omya SAS), until the pH drops to a value between 8.0 and 8.5.
• the product obtained which is a strontium carbonate of the prior art, is then dried at 140 ° C.
• This example illustrates the process according to the invention using fresh carbon dioxide.
• This test which illustrates the invention, relates to a process for producing calcium carbonate precipitated by reacting lime with fresh carbon dioxide from the combustion of ethanol from the fermentation of an organic compound such as kirsch.
• a kirsch alcohol bought in supermarkets was distilled from 37% by volume to 65% by volume and then treated with sodium sulphate to absorb the rest of the water and obtain a concentration of 97% by volume. ethanol.
• this suspension of lime formed and this alcohol obtained is introduced into the slurry of lime and at room temperature (22 ° C ⁇ 2 ° C) the fresh carbon dioxide, resulting from the combustion of the aforementioned ethanol by means of a methanol burner until the pH drops to a value between 8.0 and 8.5.
• This test which illustrates the invention, relates to a process for producing strontium carbonate by reaction of strontium hydroxide with fresh carbon dioxide from the combustion of ethanol from the fermentation of an organic compound such as kirsch .
• a kirsch alcohol bought in supermarkets was distilled from 37% by volume to 65% by volume and then treated with sodium sulphate to absorb the rest of the water and obtain a concentration of 97% by volume. ethanol.
• the product obtained which is a strontium carbonate according to the invention, is then dried at 140 ° C.
• This test which illustrates the invention, relates to a batch manufacturing process of precipitated calcium carbonate by reacting lime with fresh carbon dioxide from the fermentation of a sugar.
• This fresh carbon dioxide which is created and which is continuously formed during 21 days by the fermentation of the sugar is then introduced into the suspension of lime during these 21 days at ambient temperature (22 ° C ⁇ 2 ° C) until the pH drops to a value of about 7 ⁇ 0.3.
• This introduction of fresh carbon dioxide into the lime slurry is effected by means of a washing vessel with distilled water which collects any volatilised ethanol.
• the product obtained which is a precipitated calcium carbonate according to the invention, is then dried at 140 ° C.
• This test which illustrates the invention, relates to a continuous manufacturing process of precipitated calcium carbonate by reacting lime with fresh carbon dioxide from the fermentation of a sugar.
• an aqueous slurry of lime and fresh carbon dioxide from the fermentation of a mixture of 500 g of sucrose and 42 g of baker's yeast (saccharomyces cerevisiae) in 4 liters of water.
• an aqueous suspension of lime is first prepared by suspending 1000 g of calcium hydroxide in a vessel containing 50 liters of water without carbon dioxide and stirred by a mechanical stirrer.
• the rate of introduction of the slurry of lime corresponds to an introduction of 7.35 g in dry weight of lime per hour until 45 of the 50 liters of suspension of lime are passed through the 4 carbonation reactors.
• the fresh carbon dioxide which is created and which is continuously formed during 5 days by the fermentation of the sugar, is introduced into the 4 agitated reactors at 400 revolutions per minute and at a temperature equal to 25 ° C. ⁇ 3 ° C. during the 5 days.
• the pH in the fourth reactor has a value between 6.7 and 7.3.
• This introduction of fresh carbon dioxide into the lime slurry is effected by means of a washing vessel with distilled water which collects any volatilised ethanol.
• the product obtained, recovered in a final reservoir is a precipitated calcium carbonate according to the invention, which is then dried at 140 ° C.
• This precipitated calcium carbonate obtained is a pure calcite as shown by the infrared spectrum and has the following particle size distribution, expressed as a percentage by weight of the particles and measured with a Sedigraph TM 5100 type granulometer: 77% have a diameter ⁇ 2 ⁇ m, 44% have a diameter ⁇ 1 ⁇ m, 6% have a diameter ⁇ 0.2 ⁇ m.
• This test which illustrates the invention, relates to a process for the continuous production of a precipitated calcium carbonate obtained by reacting lime with fresh carbon dioxide resulting from the fermentation of a sugar, and then treated in a fifth reactor by sodium silicate.
• the product obtained with the same procedure as the preceding test is a precipitated calcium carbonate according to the invention, which is then treated in the fifth reactor with sodium silicate (Inosil 4237 from Van Berle), diluted in water at 1% by weight, in an amount equivalent to 4% by dry weight relative to the dry weight of calcium carbonate formed.
• the dosage was set at 0.22 g of sodium silicate per hour, corresponding to 22 ml per hour of a 1% by weight solution.
• the pH is then 10.8 ⁇ 0.1 in the fifth reactor at the end of the test.
• This test which illustrates the invention, relates to a continuous production process of a precipitated calcium carbonate obtained by reacting lime with fresh carbon dioxide from the fermentation of a sugar, and then treated in the front-end. last reactor by a sodium silicate and in the last reactor by an addition of citric acid.
• the necessary amount of citric acid is continuously added to obtain a pH of 8.5 ⁇ 0.3. It should be noted in this example, that the addition in this sixth reactor could, in an equivalent way, be carried out in batch.
• This test which illustrates the invention, relates to a process for the batch production of sodium carbonate by reacting sodium hydroxide with fresh carbon dioxide resulting from the fermentation of a sugar, and then producing a precipitated calcium carbonate. by reaction of the sodium carbonate formed according to the invention with a calcium chloride.
• This fresh carbon dioxide which is created and which is continuously formed during 21 days by the fermentation of the sugar is then introduced into the soda solution during these 21 days at ambient temperature (22 ° C. ⁇ 2 ° C.) until the pH reaches a value between 8.0 and 8.5.
• This introduction of the fresh carbon dioxide into the sodium hydroxide solution is carried out by means of a washing vessel with distilled water which collects any volatilised ethanol. Part of the solution of the sodium carbonate obtained is then filtered using a 0.45 ⁇ m filter to separate the insoluble components and obtain a filtrate which is then dried at 140 ° C. to obtain the sodium carbonate according to US Pat. 'invention.
• the sodium carbonate according to the invention is mixed at room temperature (22 ° C. ⁇ 2 ° C.) with a stoichiometric amount of calcium chloride in order to obtain a precipitated calcium carbonate whose insolubles are filtered as previously. and whose filtrate is dried at 140 ° C.
• This test which illustrates the invention, relates to a dry mixture of precipitated calcium carbonate obtained by mixing a dry calcium carbonate according to the invention (test No. 4) with a dry calcium carbonate of the prior art (Test No. 2) in a weight ratio 55/45.
• This test which illustrates the invention, relates to a dry mixture of precipitated calcium carbonate obtained by drying a mixture of a suspension of calcium carbonate according to the invention (test No. 4) with a suspension of calcium carbonate.
• calcium of the prior art (test No. 2) in a weight ratio 51/49.
• This example illustrates the process according to the invention for determining the 14 C nuclear conversion rate at 12 C of a medicinal formulation consisting essentially of calcium carbonate.
• Test No. 13 This test, which illustrates the prior art, uses a dry drug formulation consisting of a crushed natural calcium carbonate powder marketed by Omya SAS under the name of Omyapure TM. To do this, 30 mg of the test sample are placed in a 7 ml ampoule equipped with 2 consecutive 14.7 ml reactors at a pressure of 250 mbar, thus forming 2 consecutive traps, the last of which is a trap. liquid nitrogen and the first is cooled to a temperature of 20 ° C to 30 ° C above the second to avoid contamination with other volatile compounds from the sample.
• the carbon dioxide thus trapped is then reduced by hydrogenation on a cobalt powder catalyst to an elemental carbon atom ( 13 C / 12 C / 14 C).
• the nuclear conversion rate per hour and per gram of the synthetic mineral material to be analyzed is then determined by the ratio between the measured 14 C value and the value of the internationally recognized reference standard referenced in the 14 C dating methods.
• This test which illustrates the invention, implements, with the same procedure and the same material as the previous test, a dry drug formulation consisting of a calcium carbonate according to test No. 4.
• This example illustrates the use of the inorganic materials according to the invention in the paper industry as well as the method according to the invention for determining the nuclear transformation of 14 C in 12 C of a formulation in the paper industry, and more particularly in the field of offset ink.
• composition then produced is used to print an IKONOFIX TM paper, 150 g / m 2 , from M-Real TM Zanders GmbH, Bergisch-Glattbach (Germany) using a marketed "offset" printing machine. by the company SeGan (Great Britain) under the name of Ink / Surface Interaction Tester.
• ISIT Ink Surface Interaction Test
• This test is a three-phase curve: an ascending phase with a certain climb gradient, a maximum value, then a descending phase with a certain slope of descent, and is based on a printing installation provided with a device for creating and measuring the force necessary to separate a release disc, a printing ink film.
• This installation constituted on the one hand by this device for creating and measuring force and on the other hand by an ink disk rotating above the sheet of paper to be tested is marketed under the name "Ink Surface Interaction Tester" by the company SeGan Ltd.
• the paper thus coated has a value determined in g / m 2 . It is fixed on a roll equipped with a double-sided adhesive tape. The application of an offset ink is performed by contacting the ink disk with a width of 25 mm during a rotation of 180 °. The print speed and pressure are adjustable and are of the order of 0.5 m / s and 50 kg respectively. The ink volume is under standard conditions of 0.3 cm 3 thus resulting in a thickness of about 1 g / m 2 of ink on the paper sheet to be tested.
• the printing process is followed by a sequence of repeated measurements of the peeling force, at pre-selected time intervals dependent on this time set to separate this peel disc (of the same size as the printing disc) of the ink film.
• An offset printing quality nitrile rubber coating is usually used for the release disc but any equivalent material can be used.
• the contact force between the release disc and the ink is measured by a system generating an electromagnetic force.
• the amplitude and duration of the peeling force are adjusted to achieve uniform adhesion between the film surface and the peel disc after 3 seconds. Slow rotation of the paper sheet during the application of the electromagnetic force makes it possible to ensure intimate contact and continuity of the ink film.
• the peel disc retracts from the printed film by the force of a tensioned spring, sufficient force to separate the disc from the ink film.
• a strain gauge secured between the release disc and the spring, generates a signal that is recorded as the peel force.
• the sequence is automatically repeated for 13 cycles.
• the print densities are measured using a Gretag D 186 densitometer.
• the carbon dioxide thus entrapped is then reduced by hydrogenation on a cobalt powder catalyst to an elemental carbon atom ( 13 C / 12 C / 14 C).
• the isotope composition I3 C / 12 C and 15 N / 14 N of the graphite thus obtained and that of 14 C are then determined in comparison with an international reference standard by the so-called "AMS" technique for mass accelerometric mass spectrometry.
• Accelerator Mass Spectrometry "using a spectrophotometer commonly used by those skilled in the art.
• the rate of nuclear conversion per hour and per gram of the synthetic mineral material to be analyzed is then determined by the ratio between the measured 14 C value. and the value of the reference standard internationally recognized and referenced in dating methods by 14 C.
• the composition then produced is used to print a paper type IKONOFIX TM, 150 g / m 2 , from M-Real TM Zanders GmbH, Bergisch-Glattbach (Germany) using a laboratory offset printing machine. marketed by the company SeGan TM (Great Britain) under the name of Ink / Surface Interaction Tester, under the same conditions as those of the previous trial.
• SeGan TM Great Britain
• Ink / Surface Interaction Tester under the same conditions as those of the previous trial.
• the results obtained appear on curve 1 which represents the detachment force of the ink as a function of time.
• This curve is represented in drawing No. 3.
• Curve 1 shows that the offset printing of the ink, loaded with the calcium carbonate according to the invention of test No. 16 (product B of the curve 1) is identical to the offset printing of the ink, loaded with calcium carbonate according to the prior art of test No. 15 (product A of curve 1).
• This example illustrates the use of the inorganic materials according to the invention in the field of polymeric plastics, and in particular their use for the preparation of filled thermoplastic compositions such as, in particular, filled polyvinyl chloride (PVC) compositions.
• filled thermoplastic compositions such as, in particular, filled polyvinyl chloride (PVC) compositions.
• PVC polyvinyl chloride
• the charged PVC composition is produced by mixing the uncharged PVC resin and the calcium carbonate to be dispersed in a Colling TM mill equipped with two rolls of diameter equal to 150 mm and length equal to 400 mm so as to obtain a content of pigment of about 20% by weight.
• the formulation of the filled PVC composition is as follows:
• This test illustrates the invention and uses the precipitated calcium carbonate of Test No. 4 using the same procedure and equipment as the previous test.
• This test illustrates the invention and uses a mixture of 50% by weight of precipitated calcium carbonate of Test No. 4 and 50% by weight of precipitated calcium carbonate of Test No. 5 using as a coating. a polypropylene support.
• the opacity is measured according to DIN 53146 and the implementation of an Elrepho 2000 spectrophotometer from Datacolor TM AG (Switzerland).
• the so-called whiteness Tappi R 457 whiteness is determined according to TAPPI T452 ISO 247.
• Table 2 layer weight and opacity and whiteness values TAPPI R 457 measured respectively according to DIN 53146 and TAPPI T452 ISO 247
• the net values determined at a given layer weight correspond to the difference between the raw value measured for this layer weight and the raw value measured at a layer weight of 0 g / m 2 .
• the product finally obtained has a BET specific surface area equal to 52 m 2 / g.
• This BET specific surface area measurement is determined according to the BET method of the ISO 9277 standard, namely that the measurement is carried out under cooling with liquid nitrogen and under a stream of nitrogen on the dried sample until constant weight and constant temperature.
• Example 3 the same method and material as used in Example 3 are used, except for one of the two UPM TM Paper Comparative Tests.
• This test which illustrates the invention, relates to a continuous process for producing precipitated calcium carbonate by reacting lime with fresh carbon dioxide, said gas being derived from the decomposition of organic carbon source under supercritical condition.
• this test illustrates the use of one or more chemical and / or physical treatments in the manufacture of precipitated calcium carbonate according to the invention.
• an aqueous suspension is prepared having a concentration equal to 15% by dry weight of lime, stirred by means of a mechanical stirrer.
• This suspension was pumped at 238 kg / h continuously, passing two heat exchangers in a first part of the tube reactor, with a diameter of 10 to 12 mm and a second part of the tube reactor with a diameter of 6 to 8 mm.
• the Applicant indicates that the device actually has 2 heat exchangers, denoted 1 and 2.
• the product was then cooled to 16 ° C and the pressure reduced to atmospheric pressure.
• the product obtained, recovered in a final reservoir, is a precipitated calcium carbonate according to the invention, whose nuclear conversion rate of 14 C carbon at 12 C is greater than 850 transformations per hour and per gram.
• Drawing No. 6 corresponds to a photograph taken by scanning electron microscope of the product obtained.
• a second sample portion in aqueous suspension form was treated with a permanent magnetic magnet covered with Teflon.
• Drawing No. 7 corresponds to a photograph taken by scanning electron microscope of the magnet after the 5 minutes of treatment.
• a third part of the sample was ground in an aqueous medium at a concentration of 18% by dry weight of calcium carbonate, without dispersant, with zirconium oxide beads for 1 hour.
• the product obtained was then dispersed by means of sodium polyacrylate, and its particle size distribution was determined from a Sedigraph TM 5100 type apparatus: 62% by weight of the particles had a diameter of less than 2 ⁇ m and 31% by weight of the particles had a diameter of less than 1 ⁇ m.

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