WO2008012851A1 - Procédé de préparation de titanates métalliques - Google Patents

Procédé de préparation de titanates métalliques Download PDF

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Publication number
WO2008012851A1
WO2008012851A1 PCT/IT2006/000592 IT2006000592W WO2008012851A1 WO 2008012851 A1 WO2008012851 A1 WO 2008012851A1 IT 2006000592 W IT2006000592 W IT 2006000592W WO 2008012851 A1 WO2008012851 A1 WO 2008012851A1
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WIPO (PCT)
Prior art keywords
titanate
potassium
metal
materials
reaction
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PCT/IT2006/000592
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English (en)
Inventor
Mario Terruzi
Original Assignee
Immi Industria Macinazioni Minerali S.R.L.
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.)
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Publication date
Application filed by Immi Industria Macinazioni Minerali S.R.L. filed Critical Immi Industria Macinazioni Minerali S.R.L.
Priority to PCT/IT2006/000592 priority Critical patent/WO2008012851A1/fr
Priority to PCT/IB2007/002177 priority patent/WO2008012673A2/fr
Publication of WO2008012851A1 publication Critical patent/WO2008012851A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/005—Alkali titanates
    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/6261—Milling
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    • 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
    • C09C1/36—Compounds of titanium
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3215—Barium oxides or oxide-forming salts thereof
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    • 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
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/442—Carbonates
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • 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
    • C04B2235/5296—Constituents or additives characterised by their shapes with a defined aspect ratio, e.g. indicating sphericity
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • C04B2235/726—Sulfur content
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • C04B2235/727—Phosphorus or phosphorus compound content

Definitions

  • the present invention relates to a method for the preparation of metal titanates, in particular potassium titanate, as well as the titanate thus obtained, and its use as a component of materials with a high friction coefficient, in plastic materials, paints, heat resistant materials and in lubricants.
  • the typical size of the fibres of these titanate based materials relates to a length of at least 5 ⁇ m and a diameter ⁇ p to 3 ⁇ .
  • fibres of this type have also been found to be inhalable and potentially dangerous for. health.
  • each country has established the size limits for fibres used to replace asbestos according to the end products the fibres are used in, and therefore there is a rather strong need for providing new products, especially in the field of materials with a high friction coefficient; products which will not present the problems described above, and that are manufactured using materials that are within the specification limits of all countries.
  • US 5,891 ,933 describes a material with a high friction coefficient that comprises an alkaline metal titanate or alkaline earth metal titanate, such as potassium titanate for example, and a physical or chemical type binder for said titanate, such as for example a phenolic resin.
  • US 2003/0049427 describes a material with a high friction coefficient which must possess a porosity between 8 and 20% and that comprises a fibrous base' free of fibres having a length of at least 5 ⁇ m and a diameter up to 3 ⁇ m, such as for example potassium titanate, and a binder composed of a resin with specific characteristics.
  • the products obtained according to prior art are composed of titanates in the form of fibrous particles which, even when mixed with the resins as described, represent a potential problem and which are still considered as unsuitable because they are dangerous.
  • the object of the present invention is to provide a method for the preparation of metal titanates, in particular potassium titanate, which is able to form a product characterised by the rounded shape of the particles, and which is practically free of particles having an elongated form with a fibrous structure.
  • Another object of the invention to provide a method for the preparation of metal titanates, in particular potassium titanate, which is performed in solid phase and which leads to the creation of a product with round-shaped particles, and practically free of any elongated particles with a fibrous structure.
  • Another object of the present invention is to provide a metal titanate, in particular potassium titanate, characterized by round-shaped particles, and practically free of any elongated particles with a fibrous structure.
  • a further object of the present invention is to provide metal titanate, in particular potassium titanate, characterized by round-shaped particles, and practically free of any elongated particles with a fibrous structure that can be used in particular to create materials with a high friction coefficient.
  • a method for the preparation of metal titanates that includes the reaction in solid state, at a temperature between 855°C and 1200 0 C, between at least a carbonate, or hydroxide or oxide of an alkaline metal or alkaline-earth metal and a source of TiO 2 .
  • said carbonate, hydroxide or oxide is preferably chosen in the form of potassium carbonate
  • said source of TiO 2 is rutile, a mineral composed of titanium dioxide.
  • the metal titanate thus obtained is potassium titanate, in particular potassium hexatitanate in the formula
  • all metal titanates in particular, potassium titanates having the general formula x(K 2 O)y(TiO2), produced using methods according to known techniques, are characterised by an elongated crystal structure, in the form of needles and/or fibres.
  • the method according to the present invention permits the formation of a metal titanate, in particular potassium hexatitanate in the formula K 2 Ti 6 ⁇ i 3 (1 (K 2 O)6(TiO 2 ) characterised in that it possesses almost no elongated crystals in needle and/or fibre form.
  • the particles of potassium hexatitanate obtained according to the method of the invention have a rounded, almost spherical form (and are therefore defined as rounded spherical particles) presenting a ratio between length and diameter which is less than 3.
  • metal titanate, in particular potassium titanate, obtained as a raw reaction product does not contain particles with a length less than 2 ⁇ m, apart from extremely small percentages formed accidentally.
  • the particles obtained in this manner have a spherical and/or rounded ellipsoid shape, and as well as not having an elongated and therefore fibrous form, they are not flat or lenticular, and possess parameters very far from those imposed by the limits established by national and international standards.
  • the spherical and/or rounded ellipsoid form of the particle is able to guarantee that the metal titanate, and in particular, the potassium titanate according to the invention, can be considered a valid alternative to products currently on the market, and can remain in use without restraint even if the limits currently applied for the use of fibrous substances are restricted even further in the future.
  • metal titanate in particular potassium hexatitanate according to the invention
  • metal titanate can be advantageously used in materials with a high friction coefficient or other materials for example, since the rounded spherical form of its particles,- and the almost complete absence of elongated fibrous particles, whether in needle, flat or lenticular form, frees the materials in which they are used from the limits and restrictions imposed by a large number of European and international standards, thus making the material in question suitable for safe and widespread application.
  • the method for the preparation of metal titanates, in particular potassium titanate according to one of the aspects of the present invention, provides for the use of rutile in powder form and potassium carbonate or potassium hydroxide as an initial reagent.
  • Rutile powder has a nominal fineness of 325 mesh but other sizes , including sand, can be used, and this has a TiO 2 content of approximately 95%.
  • the potassium carbonate employed is obtained synthetically, and can therefore be considered as pure.
  • the initial reagents are mixed for a sufficient time in a paddle mixer, and are then sent into a hopper for loading directly or indirectly into a free-fired rotating furnace using diesel, methane gas or liquid propane gas as fuel.
  • the material can be fired continuously or in batches.
  • Furnace temperatures range between 855°C and 1200 0 C, preferably between 1000 0 C and 1200°C, and more preferably, the ideal conditions for furnace operation are at 1000°C.
  • the rutile is advantageously used in quantities that are higher than stechiometric levels.
  • the material produced is ground appropriately, for example in a ball grinder, where the choice of the type of ball and the coating is made according to the purity requirements for the finished product. This also applies to the choice of the appropriate granulometric range according to the requirements of the markets where the end products are destined.
  • the production of rounded spherical particles of potassium titanate according to the aforesaid method reaches and exceeds 99%.
  • a titanate of the formula xTiO 3 or one of its precursors to the reaction mixture, where x represents an alkaline earth metal, chosen from Mg, Ca, Sr, or Ba, for example, permits the production of an end product characterized by 100% spherical and/or ellipsoid, and/or rounded ellipsoid particles.
  • x represents an alkaline earth metal, chosen from Mg, Ca, Sr, or Ba
  • the best results were obtained by adding CaTiO 3 or the reagents that lead to its formation, to the reaction mixture.
  • the molar ratio of the end mixture CaTiO 3 / KaTi 6 Oi 3 ranges between 1 0:25/1 and 1.5/1.
  • the method according to the invention involves a mechanism which provokes the formation of a cubic structure of a Calcium titanate crystal, around which a growth of micro-crystals, also monocliriic, is formed, but which is, in any case, large enough to lead the formation of end product spherical particles, in particular potassium hexatitanate in the case described above and provided as an example.
  • the installation equipment for the production of metal titanates, in particular potassium and sodium titanates comprises the following:
  • the raw materials used for the production of potassium titanate are: rutile and potassium carbonate mineral powder.
  • the raw materials are loaded into the mixer in the following proportions: 100 Kg of K 2 CO 3 and 350 Kg of rutile for each batch, mixed until they are completely homogeneous, then unloaded into a tank with a valve at the bottom which is then loaded into the furnace.
  • the total amount of material loaded into the furnace for each batch is 450 Kg and the theoretical amount of end product is 415 Kg for each batch.
  • the amount of material normally dispersed in fumes is about 15-20 Kg for each batch.
  • the furnace is run on LPG.
  • Each batch is left to react for 3 hours at a temperature of 1100 0 C.
  • the batch is unloaded into an iron container, however it is not left to cool in these conditions, but poured onto a flat surface and spread as finely as possible so that cooling can occur very rapidly.
  • the material is cool it is ground in a hammer mill, such as a "Danioni" type, equipped with an electric 50 kw motor, producing a yield of 100 Kg/h.
  • a hammer mill such as a "Danioni" type, equipped with an electric 50 kw motor, producing a yield of 100 Kg/h.
  • another stage can be added, passing the material through a sifter with a 1 mm mesh. After grinding, the material is collected and packaged for example in bags, according to use and final destination.

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  • Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
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  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
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  • Physics & Mathematics (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé de préparation de titanates métalliques, notamment d'hexatitanate de potassium et son utilisation en tant que composant dans des matériaux présentant un coefficient de frottement élevé, dans des matériaux plastiques, des peintures, des matériaux résistants à la chaleur et des lubrifiants.
PCT/IT2006/000592 2006-07-28 2006-07-28 Procédé de préparation de titanates métalliques WO2008012851A1 (fr)

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PCT/IT2006/000592 WO2008012851A1 (fr) 2006-07-28 2006-07-28 Procédé de préparation de titanates métalliques
PCT/IB2007/002177 WO2008012673A2 (fr) 2006-07-28 2007-07-27 Procédé de préparation de titanates de métal

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PCT/IT2006/000592 WO2008012851A1 (fr) 2006-07-28 2006-07-28 Procédé de préparation de titanates métalliques

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2700626A4 (fr) * 2011-04-22 2015-04-29 Toho Material Co Ltd Procédé de fabrication d'un oxyde métallique complexe, corps fritté d'oxyde métallique et four rotatif
IT201800020470A1 (it) * 2018-12-20 2020-06-20 Mario Gerardo Terruzzi Procedimento per la preparazione di titanati alcalini esenti da fibre
IT201800020485A1 (it) * 2018-12-20 2020-06-20 Mario Gerardo Terruzzi Procedimento per la preparazione di titanato di potassio e manganese non fibroso

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108299863B (zh) * 2018-01-31 2020-12-01 攀枝花学院 一种钛白的清洁生产方法
CN116793068B (zh) * 2023-08-29 2023-10-31 常州市范群干燥设备有限公司 一种卸料结构

Citations (4)

* Cited by examiner, † Cited by third party
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US3320025A (en) * 1963-09-11 1967-05-16 Bichowsky Foord Von Process for the preparation of a titanate containing two alkali metals
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US4652439A (en) * 1984-03-12 1987-03-24 Otsuka Kagaku Kabushiki Kaisha Process for preparing fibrous alkali metal titanate
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IT201800020470A1 (it) * 2018-12-20 2020-06-20 Mario Gerardo Terruzzi Procedimento per la preparazione di titanati alcalini esenti da fibre
IT201800020485A1 (it) * 2018-12-20 2020-06-20 Mario Gerardo Terruzzi Procedimento per la preparazione di titanato di potassio e manganese non fibroso
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