CN110589889B - Inorganic composite orange pigment and preparation method thereof - Google Patents
Inorganic composite orange pigment and preparation method thereof Download PDFInfo
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- CN110589889B CN110589889B CN201910968252.6A CN201910968252A CN110589889B CN 110589889 B CN110589889 B CN 110589889B CN 201910968252 A CN201910968252 A CN 201910968252A CN 110589889 B CN110589889 B CN 110589889B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
- C01G33/006—Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
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- 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
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- 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
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- 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)
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- 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)
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- 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)
Abstract
The invention discloses an inorganic composite orange pigment, the chemical composition of which is Sn2‑xZnxTi2‑yNbyO7‑δX is more than or equal to 0.4 and less than or equal to 1.3, y is more than or equal to 0 and less than or equal to 1.0, and orange pigments with different hues can be obtained by changing the content of Zn and Nb ions. In addition, a preparation method of the inorganic composite orange pigment is also disclosed. The inorganic composite orange pigment has the advantages of uniform powder particle size, good dispersibility, environmental protection, no toxicity, bright color, strong covering power, good thermal stability, good weather resistance and the like, can completely replace the traditional cadmium orange containing heavy metal ions or iron oxide orange with poor stability, toxic organic orange pigment and the like, and can simultaneously meet the application requirements of different industries such as ceramics, glass, enamel, paint, printing ink, colored plastics and the like.
Description
Technical Field
The invention relates to the technical field of inorganic pigments, in particular to a novel environment-friendly nontoxic bright-colored inorganic composite orange pigment and a preparation method thereof.
Background
The inorganic pigment has the advantages of excellent weather resistance, temperature resistance, chemical stability and the like, and is widely applied in the fields of coloring ceramics, high-grade coatings, enamels, glass, printing ink, environment-friendly engineering plastics and the like. The common inorganic pigment varieties in the market at present mainly comprise black (such as copper chromium black and coated carbon black), red (such as cadmium red, cerium sulfide red and iron red), yellow (such as praseodymium yellow, titanium yellow, bismuth yellow and cadmium yellow), blue (such as cobalt blue) and green (such as cobalt green)Chromium green), etc., while single-phase inorganic orange pigments are less common. In practical industrial application, the inorganic orange pigment is generally prepared by mixing and blending a certain proportion of red pigment and yellow pigment, wherein cadmium orange (made of CdSe)1-xSxCdS, HgS, etc.) are most common. But commonly used cadmium Red (CdSe)1-xSx) Cadmium yellow (CdS), chrome yellow (PbCrO)4) Antimony yellow (Sb)2O52PbO) and the like, and the application of the inorganic pigment is strictly limited in the face of increasingly strict global environmental requirements. For this reason, the prior art has also developed a process for preparing iron oxide red (Fe)2O3) And iron oxide yellow (Fe)2O3·H2O) and BaSO4Fillers, etc. are mixed to form the class of iron oxide orange pigments. However, since ferrite yellow is a monohydrate (Fe) of iron oxide2O3·H2O), the pigment is converted into red color by volatilizing crystal water upon heating, and thus its thermal stability and weather resistance are poor. In addition, an orange pigment prepared by mixing inorganic red and yellow pigments in a certain ratio generally has dark color, and the color development performance of the pigment is affected. Compared with inorganic pigments, although the organic orange pigments have more types and bright colors, the organic orange pigments have poor weather resistance, temperature resistance and chemical stability, and most of the organic orange pigments have toxic or volatile carcinogenic substances, so that the applications of the organic orange pigments are also strictly limited, and the organic orange pigments are gradually replaced by environment-friendly inorganic pigments. Therefore, the development of novel environment-friendly nontoxic inorganic pigments with excellent quality to replace the traditional inorganic orange pigments containing heavy metals and toxic organic orange pigments has important significance in meeting the increasing demands for environment-friendly pigments in industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an inorganic composite orange pigment which is green, environment-friendly, bright in color and good in weather resistance to replace the traditional inorganic orange pigment containing heavy metal and toxic organic orange pigment, so that the application requirements of different industries such as ceramics, glass, enamel, paint, printing ink, colored plastics and the like are better met. Another object of the present invention is to provide a method for preparing the inorganic composite orange pigment.
The purpose of the invention is realized by the following technical scheme:
the invention provides an inorganic composite orange pigment, the chemical composition of which is Sn2-xZnxTi2-yNbyO7-δX is more than or equal to 0.4 and less than or equal to 1.3, and y is more than or equal to 0 and less than or equal to 1.0. By varying the Zn and Nb ion content, orange pigments of different shades can be obtained. The pigment has a hue value of L-60-80, a-20-35, and b-25-60.
In the scheme, x is more than or equal to 0.6 and less than or equal to 1.2, y is more than or equal to 0 and less than or equal to 0.5, reddish bright orange can be obtained, preferably, x is more than or equal to 0.8 and less than or equal to 1.0, and y is more than or equal to 0.15 and less than or equal to 0.3. X is more than or equal to 0.6 and less than or equal to 1.2, y is more than 0.5 and less than or equal to 1.0, and yellowish bright orange can be obtained, preferably, x is more than or equal to 0.8 and less than or equal to 1.0, and y is more than or equal to 0.7 and less than or equal to 0.9.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the inorganic composite orange pigment provided by the invention adopts a solid phase method, and comprises the following steps:
(1) SnO, ZnO and TiO2、Nb2O5The preparation method comprises the following steps of preparing raw materials according to chemical compositions, and uniformly mixing the raw materials through wet ball milling, wherein the ball milling rotation speed is 400-450 r/min, and the ball milling time is 4-8 h to obtain a mixed material;
(2) drying the mixed material at the temperature of 70-80 ℃ to obtain powder;
(3) putting the powder into a tubular furnace, and introducing nitrogen or argon as protective atmosphere, wherein the flow rate is 20-80 mL/min; and then heating to 750-950 ℃ at the speed of 5-10 ℃/min for sintering, keeping the temperature for 3-5 h, and naturally cooling to room temperature after sintering to obtain the inorganic composite orange pigment.
Further, in the preparation process of the solid phase method, when y is more than or equal to 0 and less than or equal to 0.5, the temperature is increased to 800-850 ℃ for sintering; and when y is more than 0.5 and less than or equal to 1.0, heating to 850-900 ℃ for sintering.
The preparation method of the inorganic composite orange pigment provided by the invention adopts a liquid phase precipitation method, and comprises the following steps:
(1) from stannous chloride (SnCl)2·2H2O), zinc nitrate (Zn (NO)3)2·6H2O), butyl titanate or titanium sulfate, niobium ethoxide or niobium pentachloride are taken as raw materials and are mixed according to chemical compositions; dissolving stannous chloride, butyl titanate and niobium ethoxide in alcohol-water mixed solution to obtain solution A; dissolving zinc nitrate in water to obtain a solution B; then adding the solution B into the solution A, and fully and uniformly mixing to obtain a mixed ion solution C; the concentration of metal ions in the mixed ion solution C is calculated according to the theory to obtain Sn2-xZnxTi2-yNbyO7-δMeter, Sn2-xZnxTi2-yNbyO7-δThe concentration of (A) is 1.0-2.0 mol/L;
(2) dissolving ammonium carbonate in an ammonia solution to obtain a precipitant solution D;
(3) dropwise adding the precipitant solution D into the mixed ion solution C until the pH value of a solution system is 8.5-10, and carrying out precipitation reaction to generate a metal ion precipitate;
(4) cleaning the metal ion precipitate with ethanol, and drying at the temperature of 60-70 ℃ to obtain powder;
(5) putting the powder into a tubular furnace, and introducing nitrogen or argon as protective atmosphere, wherein the flow rate is 20-80 mL/min; and then heating to 750-850 ℃ at the speed of 5-10 ℃/min for sintering, keeping the temperature for 3-5 h, and naturally cooling to room temperature after sintering to obtain the inorganic composite orange pigment.
Further, in the preparation process of the liquid-phase precipitation method, when y is more than or equal to 0 and less than or equal to 0.5, the temperature is increased to 750-800 ℃ for sintering; and when y is more than 0.5 and less than or equal to 1.0, heating to 800-850 ℃ for sintering.
The invention has the following beneficial effects:
(1) the inorganic composite orange pigment has the advantages of environmental protection, no toxicity, bright color, strong covering power, good thermal stability and weather resistance, and the like, can simultaneously meet the application requirements of different industries such as ceramics, glass, enamel, paint, printing ink, colored plastics, and the like, and can be completely used as a substitute of the traditional cadmium orange containing heavy metal ions or iron oxide orange with poor stability, toxic organic orange pigment, and the like.
(2) The invention controls the inorganic composite pigment Sn2-xZnxTi2-yNbyO7-δThe content of Zn and Nb in the pigment can effectively regulate and control the electronic structure (energy band structure) of the crystal formed by the pigment, improve the reflectivity of the pigment crystal phase particles to orange light, increase the absorption to green and blue light and enable the pigment to present bright orange color.
(3) The inorganic composite orange pigment composition system is suitable for synthesis preparation by a solid phase method and a liquid phase precipitation method, superfine orange pigments with average particle sizes of about 1 micron and about 0.3 micron can be obtained respectively, and pigment powder particles are uniform in size and good in dispersibility; and the color tone of the orange pigment can be further regulated and controlled by controlling the protective atmosphere and the flow rate thereof in the calcining process.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 is an SEM photograph of an inorganic composite orange pigment prepared according to one embodiment of the present invention;
FIG. 2 is an XRD spectrum of an inorganic composite orange pigment prepared in the first example of the present invention.
Detailed Description
The first embodiment is as follows:
this example is an inorganic composite orange pigment with a chemical composition of Sn1.3Zn0.7Ti1.5Nb0.5O7-δThe preparation method adopts a solid phase method and comprises the following steps:
(1) SnO, ZnO and TiO2、Nb2O5The preparation method comprises the following steps of preparing raw materials according to chemical compositions, and uniformly mixing ethanol serving as a dispersion medium by wet ball milling, wherein the ball milling rotation speed is 450r/min, and the ball milling time is 6 hours to obtain a mixed material;
(2) drying the mixed material at the temperature of 75 ℃ to obtain powder;
(3) the powder is filled in a corundum crucible and put in a tubular furnace, argon is introduced as protective atmosphere, and the flow rate is 40 mL/min; then heating to 850 ℃ at the speed of 5 ℃/min for sintering, keeping the temperature for 5h, and naturally cooling to room temperature after sintering, thus obtaining the bright-colored inorganic composite orange pigment.
The inorganic composite orange pigment prepared in this example had values of L, a, and b of 65.2, 29.7, and 46.5, respectively, and had good dispersibility of pigment particles and an average particle diameter of about 1 μm (see fig. 1). As shown in FIG. 2, the pigment obtained consisted entirely of cubic structural phases.
Example two:
the difference between the inorganic composite orange pigment and the preparation method thereof in the embodiment I is that:
1. the preparation method comprises the step (3) of heating to 800 ℃ for sintering.
2. The inorganic composite orange pigment prepared in this example had values of L, a, and b of 67.2, 29.1, and 47.7, respectively.
Example three:
the difference between the inorganic composite orange pigment and the preparation method thereof in the embodiment I is that:
1. the chemical composition of the inorganic composite orange pigment is SnZnTi1.2Nb0.8O7-δ。
2. The preparation method comprises the step (3) of heating to 850 ℃ for sintering.
3. The inorganic composite orange pigment prepared in this example had values of L, a, b of 71.4, 27.8, 58.6, respectively.
Example four:
this example is an inorganic composite orange pigment with a chemical composition of Sn1.2Zn0.8Ti1.7Nb0.3O7-δThe preparation method adopts a liquid phase precipitation method and comprises the following steps:
(1) from stannous chloride (SnCl)2·2H2O), zinc nitrate (Zn (NO)3)2·6H2O), butyl titanate and niobium pentachloride are taken as raw materials and are mixed according to chemical compositions; dissolving stannous chloride, butyl titanate and niobium pentachloride in an alcohol-water mixed solution (the volume ratio of alcohol to water is 4: 1) to obtain a solution A; adding zinc nitrateDissolving in water to obtain solution B; then adding the solution B into the solution A, and fully and uniformly mixing to obtain a mixed ion solution C; concentration of metal ions in the mixed ion solution C to obtain Sn by theoretical calculation2-xZnxTi2-yNbyO7-δMeter, Sn2-xZnxTi2-yNbyO7-δThe concentration of (A) is 1.0 mol/L;
(2) dissolving ammonium carbonate in ammonia water solution (the mass ratio of ammonium carbonate to ammonia water solution is 1: 3) to obtain precipitant solution D;
(3) dropwise adding the precipitant solution D into the mixed ion solution C until the pH value of the solution system is 10, and carrying out precipitation reaction to generate a metal ion precipitate;
(4) washing the metal ion precipitate with ethanol, and fully drying at 70 ℃ to obtain powder;
(5) the powder is filled in a corundum crucible and put in a tubular furnace, argon is introduced as protective atmosphere, and the flow rate is 40 mL/min; then heating to 800 ℃ at the speed of 5 ℃/min for calcination, keeping the temperature for 3h, and naturally cooling to room temperature after the calcination is finished to obtain the inorganic composite orange pigment.
The inorganic orange composite pigment prepared in this example had values of L, a, and b of 64.5, 30.2, and 34.5, respectively, and had good dispersibility of pigment particles and an average particle diameter of about 0.3 μm.
Claims (9)
1. An inorganic composite orange pigment, characterized in that: chemical composition Sn2-xZn x Ti y2-Nb y O7-δ，0.4≤x≤1.3、0≤yLess than or equal to 1.0; the color tone value of the pigment is 60-80, 20-35 and 25-60.
2. The inorganic composite orange pigment of claim 1, characterized in that: the content of the active carbon is more than or equal to 0.6x≤1.2、0≤y≤0.5。
3. The inorganic composite orange pigment of claim 2, characterized in that: 0.8 of≤x≤1.0、0.15≤y≤0.3。
4. The inorganic composite orange pigment of claim 1, characterized in that: the content of the active carbon is more than or equal to 0.6x≤1.2、0.5＜y≤1.0。
5. The inorganic composite orange pigment of claim 4, characterized in that: the content of the active carbon is more than or equal to 0.8x≤1.0、0.7≤y≤0.9。
6. A process for preparing the inorganic composite orange pigment of claims 1 to 5, characterized in that: adopts a solid phase method, comprising the following steps:
(1) SnO, ZnO and TiO2、Nb2O5The preparation method comprises the following steps of preparing raw materials according to chemical compositions, and uniformly mixing the raw materials through wet ball milling, wherein the ball milling rotation speed is 400-450 r/min, and the ball milling time is 4-8 h to obtain a mixed material;
(2) drying the mixed material at the temperature of 70-80 ℃ to obtain powder;
(3) putting the powder into a tubular furnace, and introducing nitrogen or argon as protective atmosphere, wherein the flow rate is 20-80 mL/min; and then heating to 750-950 ℃ at the speed of 5-10 ℃/min for sintering, keeping the temperature for 3-5 h, and naturally cooling to room temperature after sintering to obtain the inorganic composite orange pigment.
7. The method for producing an inorganic composite orange pigment according to claim 6, characterized in that: the content of the active carbon is less than or equal to 0yWhen the temperature is less than or equal to 0.5 ℃, heating to 800-850 ℃ for sintering; 0.5 < as defined aboveyAnd when the temperature is less than or equal to 1.0, heating to 850-900 ℃ for sintering.
8. A process for preparing the inorganic composite orange pigment of claims 1 to 5, characterized in that: adopts a liquid phase precipitation method, and comprises the following steps:
(1) stannous chloride, zinc nitrate, butyl titanate or titanium sulfate, niobium ethoxide or niobium pentachloride are used as raw materials, and ingredients are prepared according to chemical compositions; mixing stannous chloride and butyl titanateDissolving ester and niobium ethoxide in alcohol-water mixed solution to obtain solution A; dissolving zinc nitrate in water to obtain a solution B; then adding the solution B into the solution A, and fully and uniformly mixing to obtain a mixed ion solution C; the concentration of metal ions in the mixed ion solution C is calculated according to the theory to obtain Sn2-xZn x Ti y2-Nb y O7-δMeter, Sn2- xZn x Ti y2-Nb y O7-δThe concentration of (A) is 1.0-2.0 mol/L;
(2) dissolving ammonium carbonate in an ammonia solution to obtain a precipitant solution D;
(3) dropwise adding the precipitant solution D into the mixed ion solution C, and carrying out precipitation reaction under the condition that the pH value of a solution system is 8.5-10 to generate a metal ion precipitate;
(4) cleaning the metal ion precipitate with ethanol, and drying at the temperature of 60-70 ℃ to obtain powder;
(5) putting the powder into a tubular furnace, and introducing nitrogen or argon as protective atmosphere, wherein the flow rate is 20-80 mL/min; and then heating to 750-850 ℃ at the speed of 5-10 ℃/min for sintering, keeping the temperature for 3-5 h, and naturally cooling to room temperature after sintering to obtain the inorganic composite orange pigment.
9. The method for producing an inorganic composite orange pigment according to claim 8, characterized in that: the content of the active carbon is less than or equal to 0yHeating to 750-800 ℃ for firing when the temperature is less than or equal to 0.5; 0.5 < as defined aboveyAnd when the temperature is less than or equal to 1.0, heating to 800-850 ℃ for sintering.
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| DE10259860A1 (en) * | 2002-12-20 | 2004-07-08 | Degussa Ag | Powder mixture consisting of titanium dioxide, zinc oxide and zinc-titanium mixed oxide |
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| US3337358A (en) * | 1958-10-10 | 1967-08-22 | Vossen Jacobus Carolu Antonius | Process of manufacturing a pigment from titanium dioxide and zinc oxide |
| CN101583567A (en) * | 2007-01-12 | 2009-11-18 | 巴斯夫欧洲公司 | Pigments containing tin and rare earth elements |
| CN101041465A (en) * | 2007-04-23 | 2007-09-26 | 山东大学 | Method for preparation of niobic acid zinc nano material |
| CN103965906A (en) * | 2013-02-01 | 2014-08-06 | 常州化学研究所 | Yttrium aluminum garnet fluorescent powder material and preparation method thereof |
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