CN108219536B - Alumina-coated gamma-Ce2S3Preparation method of red pigment - Google Patents
Alumina-coated gamma-Ce2S3Preparation method of red pigment Download PDFInfo
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- 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
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract
The invention discloses an alumina-coated gamma-Ce2S3The preparation method of red pigment comprises preparing CeO coated with aluminum hydroxide by liquid phase method2And then further carrying out high-temperature vulcanization heat treatment on the precursor in a vulcanization atmosphere and an inert atmosphere to prepare the alumina-coated gamma-Ce2S3A red colorant. In addition, the product prepared by the preparation method is also disclosed. The method effectively stabilizes gamma-Ce by coating the aluminum oxide2S3The high-temperature stability of the coating modified pigment is greatly improved, and the application field of the coating modified pigment is greatly expanded; and the process is simple, the reaction is easy to control, and the preparation process and the product performance are more stable and reliable, thereby being beneficial to industrialized popularization and application.
Description
Technical Field
The invention relates to the technical field of inorganic pigments, in particular to a coated gamma-Ce pigment2S3A preparation method of a red pigment.
Background
γ~Ce2S3The dominant wavelength is about 608 nm, the color is bright red, and the color is bright and the covering power is strong; and gamma-Ce2S3S of3p→Ce5dThe electron transition has stronger absorption capacity to ultraviolet rays, so that gamma-Ce2S3Is capable of withstanding ultraviolet radiation. Meanwhile, gamma-Ce is used as2S3Safe and nontoxic, so the cadmium-selenium red pigment is the first choice pigment for replacing toxic cadmium-selenium red. However, gamma-Ce2S3The oxidative decomposition temperature of the coloring material is 350 ℃, and the coloring material is rapidly decomposed and blackened beyond the temperature, thereby affecting the application thereof at high temperature.
Therefore, at present, the coating technology is also developed to coat one or more layers of transparent high-temperature stable materials on the surface of the pigment, and the high-temperature stability of the pigment is improved by modification. In the prior art, silicon oxide, zirconium oxide or zirconium silicate is usually used as a coating layer, although for gamma-Ce2S3The high-temperature stability of the pigment is improved, but the problems of low coating rate, difficult reaction control, poor compactness of a coating layer of a product and the like still exist in the preparation process, so that the stability and the reliability of production and preparation and the stability of the product are influenced, and the disadvantages are brought to the industrial popularization and application. Therefore, research and development of a new wrapping preparation technology or a new wrapping material are urgently needed to solve the problems in the existing research and production, so that the wrapping type gamma-Ce is promoted2S3Application and development of red pigment technology.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a CeO-based coating which takes alumina as a coating layer2Alumina-coated gamma-Ce of precursor2S3The preparation method of the red pigment is used for obtaining the coated gamma-Ce through a simple, easily-controlled and stable preparation process2S3Red pigment product, thereby effectively improving gamma-Ce2S3The high-temperature stability of the pigment expands the application field of the pigment.
The purpose of the invention is realized by the following technical scheme:
the invention provides alumina-coated gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) liquid phase method for preparing coated CeO2Precipitation of precursors
(1-1) A water-soluble +3 cerium salt and a water-soluble +3 aluminum salt are added in a molar ratio Ce3+∶Al3+Dissolving the cerium salt in water at a ratio of 1-20: 1-5 to form a mixed solution of the water-soluble + 3-valent cerium salt with the concentration of 1.5-3.5 mol/L, and then adding the mixed solution into a solvent A to stir to prepare a microemulsion A, wherein the volume ratio of water to the solvent A is 1-10: 20-100;
(1-2) adding a precipitator into the solvent B, and stirring to prepare a microemulsion B; wherein, the volume ratio of the precipitator to the solvent B is 1-10: 20-100, and the components and the proportion of the solvent A and the solvent B are the same;
(1-3) mixing the microemulsion A and the microemulsion B according to the volume ratio of the solvent A to the solvent B being 1: 1, stirring, adding a demulsifier for demulsification, and obtaining the CeO coated by the aluminum hydroxide2Precipitating a precursor;
(2) preparation of coated CeO2Precursor powder
The CeO coated by the aluminum hydroxide2Precipitating the precursor, washing with water, washing with alcohol, and drying to obtain coated CeO2Precursor powder;
(3) preparation of gamma-Ce by vulcanization heat treatment2S3Red pigment
Coating the coated CeO2The precursor powder is subjected to heat treatment in a common protective atmosphere formed by a sulfuration atmosphere and an inert atmosphere to obtain the alumina-coated gamma-Ce2S3A red colorant.
Further, the water-soluble + 3-valent cerium salt is Ce (NO)3)3·6H2O、CeCl3·7H2O、Ce2(SO4)3·8H2O or Ce (Ac)3·nH2O; the water-soluble + 3-valent aluminum salt is Al (NO)3)3·9H2O、Al2(SO4)3·18H2O or AlCl3·6H2And O. The solvent A and the solvent B are mixed liquid of 2-20: 15-50: 0.5-10 of triton, cyclohexane and n-hexanol according to the volume ratio. The precipitator is strong ammonia water; the demulsifier is acetone, ethanol or isopropanol.
In the scheme, in the step (1-1), the step (1-2) and the step (1-3), the stirring time is 1-8 hours respectively.
Further, in the step (3) of the present invention, the vulcanizing atmosphere is CS2Or H2S, inert atmosphere is N2Or Ar. And (3) according to the volume ratio of the vulcanizing atmosphere to the inert atmosphere, wherein the ratio of the vulcanizing atmosphere to the inert atmosphere is 1-30: 1-300.
In the above scheme, in step (3) of the present invention, the heat treatment system is: heating to 650-1200 ℃ at a speed of 2-10 ℃/min, preserving heat for 50-600 min, and cooling to room temperature to obtain the alumina-coated gamma-Ce2S3A red colorant.
The other purpose of the invention is realized by the following technical scheme:
the invention provides a method for preparing gamma-Ce coated by using the aluminum oxide2S3The product prepared by the preparation method of the red pigment has a red value a of more than or equal to 32; the product is calcined at 600 ℃ in the air atmosphere, and the red value a of the product is more than or equal to 30 and still presents red appearance.
The invention has the following beneficial effects:
(1) the invention firstly prepares CeO wrapped by aluminum hydroxide by a liquid phase method2And then further carrying out high-temperature vulcanization heat treatment on the precursor in a vulcanization atmosphere and an inert atmosphere to prepare the alumina-coated gamma-Ce2S3A red colorant. Through the coating of the aluminum oxide, the gamma-Ce is effectively stabilized2S3The high-temperature stability of the coating modified pigment is greatly improved.
(2) The invention effectively ensures the dispersibility and the uniformity by a liquid phase method, and has simple process and easy control of reaction; by introducing the alumina, the vulcanization process is relatively stable, and the impure phase is not easy to appear, so that the preparation process and the product performance are more stable and reliable, and the method is favorable for industrialized popularization and application.
(3) The magenta value a of the pigment prepared by the invention is more than or equal to 32. The red-colored glass still presents red appearance at 600 ℃, and the red value a is more than or equal to 30, thus greatly expanding the application field of the glass.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows alumina-coated γ -Ce of the first embodiment of the present invention2S3X-ray diffraction pattern (XRD) of red pigment;
FIG. 2 shows alumina-coated γ -Ce prepared in the second embodiment of the present invention2S3Transmission Electron Microscopy (TEM) of red colorant;
FIG. 3 shows alumina-coated γ -Ce prepared in the third embodiment of the present invention2S3Transmission Electron Microscopy (TEM) of red colorants.
Detailed Description
The first embodiment is as follows:
this embodiment is an alumina coated gamma ~ Ce2S3The preparation method of the red pigment comprises the following steps:
(1) liquid phase method for preparing coated CeO2Precipitation of precursors
(1-1) 5.5g of Ce (NO)3)3·6H2O、4.5g Al(NO3)3·9H2Dissolving O in 5ml of water, then dripping into a solvent A consisting of 10ml of triton, 30ml of cyclohexane and 8ml of n-hexanol, and stirring for 4 hours at room temperature to prepare microemulsion A;
(1-2) dripping 4.5ml of strong ammonia water into a solvent B consisting of 10ml of triton, 30ml of cyclohexane and 8ml of n-hexanol, and stirring for 4 hours at room temperature to prepare a microemulsion B;
(1-3) mixing the microemulsion A and the solvent B according to the volume ratio of 1: 1Mixing the micro-emulsion B, continuously stirring for 5h at room temperature, adding acetone for demulsification to obtain CeO coated by aluminum hydroxide2Precipitating a precursor;
(2) preparation of coated CeO2Precursor powder
The above-mentioned CeO coated with aluminum hydroxide2Precipitating the precursor, washing with water, washing with alcohol, and drying to obtain coated CeO2Precursor powder;
(3) preparation of gamma-Ce by vulcanization heat treatment2S3Red pigment
Coating the above CeO2Putting the precursor powder into a porcelain boat, putting the porcelain boat into an atmosphere furnace, and introducing CS according to the volume ratio2∶N2Heating the mixed gas at a rate of 1: 10 to 1050 ℃ at a rate of 5 ℃/min, preserving the heat for 250min, and cooling to room temperature to obtain the alumina-coated gamma-Ce2S3A red colorant.
Example two:
this embodiment is an alumina coated gamma ~ Ce2S3The preparation method of the red pigment comprises the following steps:
(1) liquid phase method for preparing coated CeO2Precipitation of precursors
(1-1) 5g of CeCl3·7H2O、4g AlCl3·6H2Dissolving O in 6ml of water, then dripping into a solvent A consisting of 12ml of triton, 35ml of cyclohexane and 9ml of n-hexanol, and stirring for 4.5 hours at room temperature to prepare a microemulsion A;
(1-2) dripping 3.5ml of concentrated ammonia water into a solvent B consisting of 12ml of triton, 35ml of cyclohexane and 9ml of n-hexanol, and stirring at room temperature for 4.5 hours to prepare a microemulsion B;
(1-3) mixing the microemulsion A and the microemulsion B according to the volume ratio of the solvent A to the solvent B being 1: 1, continuously stirring for 4.5 hours at room temperature, adding ethanol for demulsification, and obtaining CeO coated by aluminum hydroxide2Precipitating a precursor;
(2) preparation of coated CeO2Precursor powder
The above-mentioned CeO coated with aluminum hydroxide2Precipitating the precursor, washing with water, washing with alcohol, and drying to obtain coated CeO2Precursor ofBulk powder material;
(3) preparation of gamma-Ce by vulcanization heat treatment2S3Red pigment
Coating the above CeO2Putting the precursor powder into a porcelain boat, putting the porcelain boat into an atmosphere furnace, and introducing CS according to the volume ratio2Heating the mixed gas with the ratio of Ar to Ar being 1: 8 to 1000 ℃ at the speed of 5 ℃/min, preserving the heat for 360min, and cooling to room temperature to obtain the alumina-coated gamma-Ce2S3A red colorant.
Example three:
this embodiment is an alumina coated gamma ~ Ce2S3The preparation method of the red pigment comprises the following steps:
(1) liquid phase method for preparing coated CeO2Precipitation of precursors
(1-1) 5g of CeCl3·7H2O、5g Al(NO3)3·9H2Dissolving O in 6ml of water, then dripping into a solvent A consisting of 9.5ml of triton, 32ml of cyclohexane and 8ml of n-hexanol, and stirring for 7 hours at room temperature to prepare a microemulsion A;
(1-2) dripping 4ml of concentrated ammonia water into a solvent B consisting of 9.5ml of triton, 32ml of cyclohexane and 8ml of n-hexanol, and stirring for 7 hours at room temperature to prepare a microemulsion B;
(1-3) mixing the microemulsion A and the microemulsion B according to the volume ratio of the solvent A to the solvent B being 1: 1, continuing stirring for 5 hours at room temperature, adding isopropanol for demulsification, and obtaining CeO coated by aluminum hydroxide2Precipitating a precursor;
(2) preparation of coated CeO2Precursor powder
The above-mentioned CeO coated with aluminum hydroxide2Precipitating the precursor, washing with water, washing with alcohol, and drying to obtain coated CeO2Precursor powder;
(3) preparation of gamma-Ce by vulcanization heat treatment2S3Red pigment
Coating the above CeO2Putting the precursor powder into a porcelain boat, putting the porcelain boat into an atmosphere furnace, and introducing CS according to the volume ratio2∶N2Heating to 950 deg.C at 2 deg.C/min under the condition of mixed gas 1: 9, maintaining the temperature for 400min, and cooling to room temperatureThen the alumina coated gamma-Ce is prepared2S3A red colorant.
As shown in FIG. 1, the coated gamma-Ce prepared by the embodiment of the invention2S3The red pigment is composed of gamma-Ce2S3And alumina.
FIGS. 2 and 3 show that the coated gamma-Ce prepared by the embodiment of the invention2S3A red pigment composed of gamma-Ce2S3And a transparent and compact alumina wrapping layer wrapped on the surface of the glass fiber.
The alumina coated gamma-Ce prepared by the embodiments of the invention2S3The chromatic values of the red coloring materials are shown in Table 1.
TABLE 1 aluminum oxide-coated gamma-Ce of the examples of the present invention2S3Chroma value of red pigment
With uncoated commercial gamma-Ce2S3The pigment is used as a comparative example, and the alumina coated gamma-Ce prepared in the first embodiment of the invention2S3The colorimetric values of the red coloring material after firing in the air atmosphere are shown in Table 2.
TABLE 2 chroma values after calcination in air atmosphere for inventive example one and comparative example
Claims (6)
1. Alumina-coated gamma-Ce2S3The preparation method of the red pigment is characterized by comprising the following steps:
(1) liquid phase method for preparing coated CeO2Precipitation of precursors
(1-1) A water-soluble +3 cerium salt and a water-soluble +3 aluminum salt are added in a molar ratio Ce3+∶Al3+Dissolving the cerium salt in water at a ratio of 1-20: 1-5 to form a mixed solution of the water-soluble + 3-valent cerium salt with a concentration of 1.5-3.5 mol/L(ii) a Then adding the mixed solution into a solvent A and stirring to prepare a microemulsion A; wherein, the volume ratio of water to the solvent A is 1-10: 20-100, and the solvent A is a mixed solution of triton, cyclohexane and n-hexanol in a volume ratio of 2-20: 15-50: 0.5-10;
(1-2) adding a precipitator into the solvent B, and stirring to prepare a microemulsion B; wherein, the volume ratio of the precipitator to the solvent B is 1-10: 20-100, and the composition and the proportion of the solvent B are the same as those of the solvent A;
(1-3) mixing the microemulsion A and the microemulsion B according to the volume ratio of the solvent A to the solvent B being 1: 1, stirring, adding a demulsifier for demulsification, and obtaining the CeO coated by the aluminum hydroxide2Precipitating a precursor;
(2) preparation of coated CeO2Precursor powder
The CeO coated by the aluminum hydroxide2Precipitating the precursor, washing with water, washing with alcohol, and drying to obtain coated CeO2Precursor powder;
(3) preparation of gamma-Ce by vulcanization heat treatment2S3Red pigment
Coating the coated CeO2The precursor powder is subjected to heat treatment in a common protective atmosphere formed by a vulcanizing atmosphere and an inert atmosphere, namely, the temperature is increased to 650-1200 ℃ at the speed of 2-10 ℃/min, the temperature is kept for 50-600 min, and then the precursor powder is cooled to room temperature to prepare the coating gamma-Ce with the coating layer being crystalline alumina2S3The red pigment has a red value a of more than or equal to 32, and is still red in appearance after being calcined at 600 ℃ in an air atmosphere.
2. The alumina-coated γ -Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: the water-soluble + 3-valent cerium salt is Ce (NO)3)3·6H2O、CeCl3·7H2O、Ce2(SO4)3·8H2O or Ce (Ac)3·nH2O; the water-soluble + 3-valent aluminum salt is Al (NO)3)3·9H2O、Al2(SO4)3·18H2O or AlCl3·6H2O。
3. The alumina-coated γ -Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: the precipitator is strong ammonia water; the demulsifier is acetone, ethanol or isopropanol.
4. The alumina-coated γ -Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: in the step (1-1), the step (1-2) and the step (1-3), the stirring time is 1-8 hours respectively.
5. The alumina-coated γ -Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: in the step (3), the vulcanizing atmosphere is CS2Or H2S, inert atmosphere is N2Or Ar.
6. The alumina-coated γ -Ce of claim 52S3The preparation method of the red pigment is characterized by comprising the following steps: and (3) according to the volume ratio of the vulcanizing atmosphere to the inert atmosphere, wherein the ratio of the vulcanizing atmosphere to the inert atmosphere is 1-30: 1-300.
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| CN109456618B (en) * | 2018-12-24 | 2020-10-16 | 景德镇陶瓷大学 | Crystalline silicon dioxide coated gamma-Ce2S3Red pigment and preparation method thereof |
| CN112175416B (en) * | 2020-09-25 | 2021-11-23 | 景德镇陶瓷大学 | Preparation method of superfine cristobalite in-situ coated gamma-Ce 2S3 bright red pigment and product prepared by preparation method |
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