WO2006067799A1 - Procede pour la preparation de colorants inorganiques a partir de composes de terre rare melanges - Google Patents

Procede pour la preparation de colorants inorganiques a partir de composes de terre rare melanges Download PDF

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Publication number
WO2006067799A1
WO2006067799A1 PCT/IN2004/000406 IN2004000406W WO2006067799A1 WO 2006067799 A1 WO2006067799 A1 WO 2006067799A1 IN 2004000406 W IN2004000406 W IN 2004000406W WO 2006067799 A1 WO2006067799 A1 WO 2006067799A1
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WO
WIPO (PCT)
Prior art keywords
rare earth
range
mixed
mixture
group
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Application number
PCT/IN2004/000406
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English (en)
Inventor
Kalarical Janardhanan Sreeram
Balachandran Unni Nair
Thirumalachari Ramasami
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Council Of Scientific And Industrial Research
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Priority to PCT/IN2004/000406 priority Critical patent/WO2006067799A1/fr
Publication of WO2006067799A1 publication Critical patent/WO2006067799A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0009—Pigments for ceramics
    • 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
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/241—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion containing two or more rare earth metals, e.g. NdPrO3 or LaNdPrO3
    • 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
    • C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7767—Chalcogenides
    • C09K11/7769—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—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
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62—L* (lightness axis)
    • 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
    • C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
    • 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
    • C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)

Definitions

  • the present invention relates to a process for the preparation of inorganic colourants from mixed rare earth compounds. More particularly, the present invention provides a process for preparation of inorganic colourants from mixed rare earth compounds without separating individual rare earth elements present therein.
  • the invention has enormous application in colourant industry to manufacture environment friendly, non- carcinogenic and cost effective colorant.
  • the process also provides an economical option to the ore industry to use the mixed rare earth compounds for producing environmentally safe colorants.
  • Inorganic colorants contain various types of metal ions in the form of carbonates, sulfides and oxides. The nature of the metal ion plays a vital role in the color of the colorant. Several colorants conventionally used in the paint industry are toxic. These include barium chromate, cadmium sulfide, lead antimoniate etc. Regulations in Europe concerning the protection of the environment have forced the paint industry to invest heavily in research programs on development of inorganic paints that are free of heavy metals such as lead, mercury, cadmium, antimony, arsenic, chromium, selenium etc. Rare earth elements offer a vast opportunity for development of environmentally secure alternatives for many of the eco- constrained colorants.
  • Some rare earth oxides are being widely used in ceramic industry to produce colors. Sulcova et al (Dyes and Pigments, vol. 40, p87, 1998 and Dyes and Pigments, vol.47, p285, 2000) have employed cerium oxide to develop an opaque white color and by doping cerium with praseodymium, neodymium, yttrium the other different shades like yellow, violet, orange and burgundy have been obtained.
  • the ratio of R (the rare earth ion) becomes increasingly relevant with the color being dependent on the type of rare earth oxide used.
  • R the rare earth ion
  • the main objective of the present invention is to provide a novel process for the preparation of inorganic colourants from mixed rare earth compounds, which obviates the limitations as stated above.
  • Another objective of the present invention is to provide for an environmentally safe inorganic colorant whereby the use of harmful metal ions likes lead, chromium, cadmium, mercury etc are avoided.
  • Yet another objective of the present invention is to bring about charge transfer interactions and conduction band energy transfer interactions between the mixed rare earth compound and one or more metal ion.
  • the present invention provides a novel process for the preparation of inorganic colourants from mixed rare earth compounds, which comprises i) homogenising mixed rare earth compounds selected from one or more of oxide, carbonate, nitrate, fluoride, chloride of rare earth elements having atomic number in the range of 57 to 71 and having a composition of at least Cerium in the range of 40- 45%w/w, Praseodymium in the range of 4-6% w/w, Lanthanum in the range of 15- 25%, Neodymium in the range of 15-20% and other rare earths to a maximum of 5%, optionally mixed with not more than 40 times by weight of a compound of a metal ion selected from the group consisting of transition metal series, lanthanide/actinide series, group(III) or group(IV) of the periodic table, and/or not more than 0.2 times by weight of neutral salt either in liquid phase or solid state to obtain a homogenate; ii) heating the homogenate obtained in step (i), followed by cooling and
  • the homogenate is heated in step (ii) to a temperature in the range of 600 - 1800 0 C for a period of 10 - 600 minutes either continuously or with intermittent sintering.
  • the cooling in step (ii) is carried out to a temperature in the range of 35-15O 0 C.
  • the particle size in step (ii) is reduced to not more than 100 microns.
  • the rare earth element present in the mixed rare earth compound is selected from the group consisting of lanthanum, samarium, neodymium, terbium and any combination thereof.
  • the metal is selected from the group consisting of Nickel, Cobalt, Titanium, Zirconium, Aluminium, Silcon, Germanium, Thalium and any combination thereof.
  • the neutral salt used is selected from the group consisting of chloride, fluoride, phosphate and sulfate salts of sodium either individually or in any combination thereof.
  • the reduction of particle size is effected using a ball mill, grinder, crusher, attrition mill or mortar and pestle.
  • the present invention provides a novel process for the preparation of inorganic colourants from mixed rare earth compounds.
  • the process comprises
  • Neodymium in the range of 15-20% and other rare earths to a maximum of 5% optionally mixed with not more than 40 times by weight of a compound of a metal ion selected from the group consisting of transition metal series, lanthanide/actinide series, group(III) or group(IV) of the periodic table, and/or not more than 0.2 times by weight of neutral salt either in liquid phase or solid state to obtain a homogenate; iii) heating the homogenate obtained in step (i), followed by cooling and subsequent reduction of particle size of the resulting product to obtain inorganic colourants.
  • a compound of a metal ion selected from the group consisting of transition metal series, lanthanide/actinide series, group(III) or group(IV) of the periodic table
  • step (ii) The homogenate is heated in step (ii) to a temperature in the range of 600 - 1800 0 C for a period of 10 - 600 minutes either continuously or with intermittent sintering and the cooling is carried out to a temperature in the range of 35-15O 0 C.
  • the particle size in step (ii) is reduced to not more than 100 microns.
  • the rare earth element present in the mixed rare earth compound is selected from the group consisting of lanthanum, samarium, neodymium, terbium and any combination thereof.
  • the metal is selected from the group consisting of Nickel, Cobalt, Titanium, Zirconium, Aluminium, Silcon, Germanium, Thalium and any combination thereof.
  • the neutral salt used is selected from the group consisting of chloride, fluoride, phosphate and sulfate salts of sodium either individually or in any combination thereof.
  • the reduction of particle size is effected using a ball mill, grinder, crusher, attrition mill or mortar and pestle.
  • Mixed rare earth compound selected from one or more among but not limited to oxide, carbonate, nitrate, fluoride, chloride of rare earth element and having a composition of at least Cerium in the range of 40-45%w/w, Praseodymium in the range of 4-6% w/w,
  • Neodymium in the range of 15-20% and other rare earths to a maximum of 5%, optionally mixed with not more than 40 times by weight of a compound of a metal ion selected from transition metal series, lanthanide/actinide series, group(i ⁇ ) or group(IV) of the periodic table, and/or not more than 0.2 times by weight of neutral salt is homogenised either in liquid phase or solid state by known method.
  • the resulting homogenate is heated to a temperature in the range of 600 - 1800 0 C either continuously or with intermittent sintering.
  • the resulting mixture is allowed to cool down to a temperature in the range of 35-15O 0 C and the product is subjected to the reduction of particle size at a range of 1-100 microns by known method to obtain inorganic colourants.
  • the colour values are measured on the CIE scale (The CHE is short for Commission Internationale de l'Eclairage which is the French title of the international commission on light), represented by L a* b*.
  • the L-axis is known as the lightness and extends from 0 (black) to 100 (white).
  • the other two coordinates a* and b* represent redness-greeness and yellowness-blueness respectively.
  • the inventive step of the present invention lies in the use of the mixed rare earth compound as such, without subjecting the same to any separation for any specific element for subsequent compounding for colouration, thereby reducing the cost of the raw material for the production of the colourants.
  • Example 3 I g of mixed rare earth carbonate was mixed with 0.1 g of vanadyl sulfate and 0.05 g of sodium phosphate and the resultant mixture was ground to achieve a homogeneous mixture. This mixture was then heated at 1300 0 C for 2 hrs in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 5°C/min. The heated mixture was then cooled to 5O 0 C, ground in an attrition mill to reduce its particle size to 75 microns. The obtained colorant had L a* b* values of 52.13, 13.33, 16.94 respectively on the CIE scale.
  • 0.15 g of mixed rare earth carbonate was mixed with 3.2 g of aluminium sulfate and 0.32 g of chromium sulfate, and the resultant mixture ground to achieve a homogeneous mixture.
  • This mixture was then heated at 125O 0 C for 2 hrs in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 14°C/min. The heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 10 microns. The obtained colorant had whitish pink color.
  • 0.15 g of mixed rare earth carbonate was mixed with 3.2 g of aluminium sulfate and 0.21 g of manganous sulfate, and the resultant mixture ground to achieve a homogeneous mixture.
  • This mixture was then heated at 125O 0 C for 2 hrs in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 14°C/min.
  • the heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 10 microns.
  • the obtained colorant had light brown color.
  • 0.15 g of mixed rare earth carbonate was mixed with 3.4 g of aluminium sulfate, 0.2 g of copper sulfate, 0.05 g of cobaltous acetate and 0.02 g of sodium fluoride was mixture ground to achieve a homogeneous mixture.
  • This mixture was then heated at 125O 0 C for 2 hrs in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 1 l°C/min. The heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 50 microns.
  • the obtained colorant had a dark blue color.
  • Example 15 0.15 g of mixed rare earth fluoride was mixed with 3.4 g of aluminium sulfate and 0.2 g of copper sulfate and 0.05 g of cobaltous acetate, and the resultant mixture ground to achieve a homogeneous mixture. This mixture was then heated at 145O 0 C for 6 hrs in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 7°C/min. The heated mixture was then cooled to 9O 0 C, ground in a ball mill to reduce its particle size to 100 microns. The obtained colorant had a dark blue color.
  • 0.15 g of mixed rare earth fluoride was mixed with 3.4 g of aluminium sulfate and 0.2 g of copper sulfate and 0.05 g of cobaltous acetate, and the resultant mixture ground to achieve a homogeneous mixture.
  • This mixture was then heated at 145O 0 C for 30 min in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 7°C/min. The heated mixture was then cooled to 4O 0 C, ground in an attrition mill to reduce its particle size to 40 microns.
  • the obtained colorant had a blue color.
  • Example 17 1.0 g of mixed rare earth fluoride was mixed with 0.1 g of barium carbonate, and the resultant mixture ground to achieve a homogeneous mixture. This mixture was then heated at 1000 0 C for 30 min in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 2°C/min. The heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 100 microns. The obtained colorant had a brown color.
  • Example 18 1.0 g of mixed rare earth fluoride was mixed with 0.1 g of barium carbonate, and the resultant mixture ground to achieve a homogeneous mixture. This mixture was then heated at 1000 0 C for 30 min in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 2°C/min. The heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 100 microns. The obtained colorant had a brown color.
  • 0.70 g of mixed rare earth nitrate was mixed with 0.24 g of nickel carbonate and 2.2 g of zinc sulfate and the resultant mixture ground to achieve a homogeneous mixture.
  • This mixture was then heated at 1200 0 C for 90 min in a refractory furnace in the presence of atmospheric oxygen. The rate of heating was maintained at 10°C/min.
  • the heated mixture was then cooled to 4O 0 C, ground in a ball mill to reduce its particle size to 10 microns.
  • the obtained colorant had a green color.
  • the prepared colorant by suitable doping of mixed rare earth carbonate can generate colors with similar L a b values on the CEE scale.
  • the L a b values of the colorant in example 23 has a similar L a b value as that of a colorant having the fixed composition of CeC 70 Pr 0- O 5 La 0-25 0 L 875 ' which has been prepared by independent mixing of cerium oxide, praseodymium oxide, and lanthanum oxide (L a b values of 65.43, 20.78 and 23.87 respectively).
  • the covering properties of these colorants are similar. Advantages
  • This process provides a route to the preparation of inorganic colorants of varying hues and colors by the use of mixed rare earth compounds, thereby obviating the need for separation of the individual rare earth elements 2.
  • This process makes use of a mixed rare earth compound, which therefore reduces the cost of preparation of the colorant by 10-100 times 3.
  • This process depends on mixed rare earth compounds, which are environmentally safe than the conventional colorants based on mercury, lead, cadmium etc.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

La présente invention fournit un nouveau procédé pour la préparation de colorants inorganiques à partir de composés de terre rare mélangés, lesquels sont directement obtenus auprès de l'industrie minière, sans subir une quelconque séparation, permettant de ce fait une réduction des coûts dans un rapport de 10 à 100. Des couleurs dans la gamme de marron, bleu et vert peuvent être obtenues en ajoutant d'autres ions métalliques.
PCT/IN2004/000406 2004-12-24 2004-12-24 Procede pour la preparation de colorants inorganiques a partir de composes de terre rare melanges WO2006067799A1 (fr)

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PCT/IN2004/000406 WO2006067799A1 (fr) 2004-12-24 2004-12-24 Procede pour la preparation de colorants inorganiques a partir de composes de terre rare melanges

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PCT/IN2004/000406 WO2006067799A1 (fr) 2004-12-24 2004-12-24 Procede pour la preparation de colorants inorganiques a partir de composes de terre rare melanges

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010109493A1 (fr) * 2009-03-27 2010-09-30 Council Of Scientific & Industrial Research Preparation de colorant vert a partir de terres rares mixtes et de composes de molybdene et traitement de revêtements de surfaces associes

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0654507A1 (fr) * 1993-11-18 1995-05-24 Rhone-Poulenc Chimie Pigments à base d'oxyde de zirconium et de cérium, de praséodyme et/ou de terbium, leur procédé de préparation et leur utilisation
US20020034644A1 (en) * 2000-06-07 2002-03-21 Swiler Daniel R. Rare earth-transition metal oxide pigments

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0654507A1 (fr) * 1993-11-18 1995-05-24 Rhone-Poulenc Chimie Pigments à base d'oxyde de zirconium et de cérium, de praséodyme et/ou de terbium, leur procédé de préparation et leur utilisation
US20020034644A1 (en) * 2000-06-07 2002-03-21 Swiler Daniel R. Rare earth-transition metal oxide pigments

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
S.P. SIMNER, J.S. HARDY, J.W. STEVENSON: "Sintering and Properties of Mixed Lanthanide Chromites", J. ELECTROCHEM. SOC., vol. 148, no. 4, 2001, pages A351 - A360, XP002348980 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010109493A1 (fr) * 2009-03-27 2010-09-30 Council Of Scientific & Industrial Research Preparation de colorant vert a partir de terres rares mixtes et de composes de molybdene et traitement de revêtements de surfaces associes
CN102414129A (zh) * 2009-03-27 2012-04-11 科学与工业研究委员会 由混合稀土及钼化合物制备绿色着色剂及其表面涂布方法
JP2012521946A (ja) * 2009-03-27 2012-09-20 カウンスィル オブ サイエンティフィック アンド インダストリアル リサーチ 混合希土類化合物およびモリブデン化合物からの緑色着色料の製造およびその表面コーティング方法
CN102414129B (zh) * 2009-03-27 2014-07-30 科学与工业研究委员会 由混合稀土及钼化合物制备绿色着色剂及其表面涂布方法
US9242872B2 (en) 2009-03-27 2016-01-26 Council Of Scientific & Industrial Research Preparation of green colorant from mixed rare earth and molybdenum compounds and process of surface coatings thereof

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