CN112625464B - Preparation method of PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce 2S3 red pigment and product prepared by preparation method - Google Patents
Preparation method of PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce 2S3 red pigment and product prepared by preparation method Download PDFInfo
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Abstract
The invention discloses PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce2S3Preparation method of red pigment, which takes cerium source solution and silicon source solution containing PEG as raw materials to prepare CeO2@a‑SiO2Wrapping precursor powder; then adding carbon powder before or after the vulcanization treatment for treatment, and sintering to obtain the superfine cristobalite coated gamma-Ce2S3A red colorant. In addition, the product prepared by the preparation method is also disclosed. The preparation method can obtain cristobalite-coated gamma-Ce with fine particles, good dispersibility and stable suspension in the solvent2S3Red pigment, thereby widening gamma to Ce2S3The application field of red pigment is favorable for promoting the coating type gamma-Ce2S3The application of the pigment in the actual production.
Description
Technical Field
The invention relates to the technical field of inorganic pigments, in particular to ultrafine cristobalite coated gamma-Ce2S3A preparation method of a red pigment and a product prepared by the method.
Background
γ～Ce2S3Because of the characteristics of bright red color, strong ultraviolet resistance, environmental protection, no toxicity and the like, the red pigment becomes the best substitute of a heavy metal-containing scarlet pigment, namely a cadmium selenium red pigment, and is widely used in the fields of plastic production, printing ink, vehicle paint and the like. However, Ce3+Strong oxygen affinity, can be oxidized to lose red color at 350 ℃ in air atmosphere, and limits gamma-Ce2S3In the field of high temperature, Thierry proposes to coat a layer of colorless and transparent SiO with good chemical stability and high temperature resistance on the surface of the pigment2、 ZrO2Or ZrSiO4Can improve the thermal stability, chemical corrosion resistance and dispersibility of the product under the condition that the color of the product is not affected basically, namely, the product is gamma-Ce2S3The surface is coated with a layer of wrapping layer to form a core-shell structure, so that the purpose of isolating oxygen is achieved, and the oxidation resistance temperature of the coating is further improved.
At present, researchers and researchers adopt hydrothermal method, hydrolysis method, sol-gel method, microemulsion method and other methods to prepare SiO2、 ZrSiO4、ZnO、MgAl2O4Coated gamma-Ce as coating layer2S3The red pigment, although the oxidation resistance temperature and the chemical stability of the pigment are improved, still has the problems of serious agglomeration, large particles, poor dispersibility and the like of the coating pigment, and the prepared coating pigment cannot be used in actual production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of red pigment is used for obtaining cristobalite-coated gamma-Ce with fine particles, good dispersibility and stable suspension in solvent2S3Red pigment, thereby widening gamma to Ce2S3The application field of red pigment, namely encapsulated gamma-Ce2S3The colorant can be applied to actual production. The invention also aims to provide cristobalite-coated gamma-Ce refined by utilizing the PEG and the carbon powder2S3The product is prepared by the preparation method of the red pigment.
The purpose of the invention is realized by the following technical scheme:
the invention provides PEG and carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) preparation of the stock solution
Cerium source solution: according to the molar ratio Ce3+∶H+Urea and alkali metal ions in a ratio of 1-4: 2-5: 6-12: 0.05-0.8, dissolving soluble cerium salt, acid, Urea and an alkali metal ion source in an alcohol-water mixed solution, and uniformly mixing to obtain a cerium source solution;
silicon source solution: dissolving tetraethyl orthosilicate and PEG (polyethylene glycol) in absolute ethyl alcohol according to the mass ratio of tetraethyl orthosilicate to absolute ethyl alcohol to PEG of 1: 3-10: 0.6-3 to obtain a silicon source solution;
(2)CeO2@a-SiO2preparation of coated precursor powder
(2-1) according to the molar ratio Si4+∶Ce3+Pouring the silicon source solution into the cerium source solution, stirring and mixing uniformly, and adding acid to adjust the pH value to obtain an acidic precursor solution, wherein the ratio of the silicon source solution to the cerium source solution is 5-15: 1-3;
(2-2) carrying out acid catalysis treatment on the precursor solution to form transparent acid catalysis gel, then carrying out heating treatment to form white base catalysis gel, drying and grinding to obtain precursor powder;
(2-3) calcining the precursor powder at the temperature of 150-1000 ℃ for 1-100 min to remove the coating on SiO2After PEG on the surface layer, the superfine CeO is obtained by grinding2@a-SiO2Coating the precursor powder of a-SiO2Is amorphous SiO2；
(3) gamma-Ce treated with carbon powder2S3@a-SiO2Preparation of
According to mass ratio of CeO2@a-SiO21: 0.05-2 of carbon powder, and mixing the CeO2@a-SiO2Mixing and grinding the wrapped precursor powder and carbon powder, calcining at the temperature of 600-800 ℃ for 60-120 min, and then carrying out vulcanization treatment in the atmosphere of inert vulcanization gas to obtain gamma-Ce treated by carbon powder2S3@a-SiO2；
Or, the CeO is added2@a-SiO2The wrapped precursor powder is vulcanized in the atmosphere of inert vulcanizing gas to obtain gamma-Ce2S3@a-SiO2Then according to the mass ratio of gamma to Ce2S3@a-SiO21: 0.05-2 of carbon powder, and mixing the gamma-Ce2S3@a-SiO2Mixing and grinding with carbon powder to obtain gamma-Ce treated by carbon powder2S3@a-SiO2；
(4) Cristobalite-coated gamma-Ce2S3Preparation of
Treating the gamma-Ce treated with the carbon powder2S3@a-SiO2Calcining in inert gas atmosphere, acid washing the calcined product, and air atmosphereCalcining to obtain superfine gamma-Ce with the average particle size of 3.8-4.6 mu m2S3@c-SiO2A coated red pigment of c-SiO2Is cristobalite.
Furthermore, the polymerization degree of the PEG is 600-20000. And (3) the pH value of the precursor solution in the step (2-1) is 2-3.
Further, in the step (2-2), acid catalysis treatment is carried out for 12-24 hours at the temperature of 50-60 ℃; and treating the transparent acid catalysis gel at the temperature of 80-100 ℃ for 48-72 h to form white alkali catalysis gel. The temperature of the vulcanization treatment in the step (3) is 800-1100 ℃, and the vulcanization time is 60-180 min. The calcination temperature of the step (4) in the inert gas atmosphere is 1250-1400 ℃, and the calcination time is 60-180 min; the calcination temperature in the air atmosphere is 400-700 ℃, and the calcination time is 30-100 min.
Cristobalite-coated gamma-Ce refined by utilizing PEG and carbon powder2S3The product prepared by the preparation method of the red pigment comprises a cristobalite matrix and gamma-Ce coated in the matrix2S3Pigment particles of a chroma value L*＝35.43～40.54、a*＝32.86～37.54、b*23.90-32.84; calcining at 500-900 ℃ in air atmosphere to obtain red pigment with a chromatic value L*＝33.14～42.53、a*＝28.56～37.31、b*＝ 23.94～32.48。
The invention has the following beneficial effects:
(1) the invention adopts PEG as a cross-linking agent for the first time and SiO generated by hydrolysis of TEOS2A crosslinking effect is formed, thereby controlling SiO2Particle size of (2) prevents the formation of large SiO in the polycondensation process of the hydrolysis product2And (3) performing agglomeration, drying and calcining the obtained precursor to remove PEG crosslinked between CeO2@ a-SiO2 particles, and obtaining the superfine CeO2@ a-SiO2 pigment precursor.
(2) According to the invention, carbon powder is added before or after vulcanization treatment to serve as a spatial resistance agent, the influence of carbon powder with different addition amounts on preventing agglomeration and color development of the wrapped pigment during high-temperature calcination is firstly researched, and the influence of carbon powder with different addition amounts on the prevention of agglomeration and color development of the wrapped pigment is firstly researchedPreparing superfine gamma-Ce with average grain diameter of 4 mu m2S3@c-SiO2And (5) coating a pigment. The cristobalite coated gamma-Ce obtained by the invention2S3The pigment has fine particles, good dispersibility in water and various organic solvents, and can form stable suspension in the solvent, thereby being beneficial to widening gamma-Ce2S3The application field of red pigment, namely encapsulated gamma-Ce2S3The colorant can be applied to actual production.
(3) The preparation process of the invention has simple operation, low requirement on production equipment, wide application range of products and easy popularization to the preparation of other coating pigments. In addition, the invention not only improves the product quality of the finished pigment, but also can well adapt to the development trend of environment-friendly and clean production, and is beneficial to the development and popularization of the production technology of the silicon dioxide coated pigment.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows cristobalite-coated gamma-Ce prepared in the first embodiment of the present invention2S3Particle size distribution of red pigment;
FIG. 2 shows cristobalite-coated gamma-Ce prepared in the example of the present invention2S3Transmission images of red coloring materials (a: TEM image; b: HR-TEM image).
Detailed Description
The first embodiment is as follows:
this example is PEG, carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) preparation of the stock solution
Cerium source solution: according to the molar ratio Ce3+∶H+∶Urea∶Na+At 4: 2: 10: 0.2, adding Ce (NO)3)3· 6H2O, nitric acid, urea, NaNO3Dissolving in alcohol-water mixture with volume ratio of ethanol to water of 1.5: 1, and mixing to obtain Na+An ion-doped cerium source solution;
silicon source solution: tetraethyl orthosilicate and PEG are dissolved in absolute ethyl alcohol according to the mass ratio of 1: 3: 1.2 to obtain a silicon source solution;
(2)CeO2@a-SiO2preparation of coated precursor powder
(2-1) according to the molar ratio Si4+∶Ce3+Pouring the silicon source solution into the cerium source solution, stirring and mixing uniformly, adding nitric acid to adjust the pH value to 2, and stirring for 60min under a magnetic stirrer with the rotating speed of 300r/min to obtain a precursor solution;
(2-2) carrying out acid catalysis treatment on the precursor solution in a drying oven at the temperature of 55 ℃ for 24 hours to form transparent acid catalysis gel, then putting the acid catalysis gel into the drying oven to react at the temperature of 80 ℃ for 48 hours to hydrolyze urea to obtain white base catalysis gel, further drying at the temperature of 80 ℃ and then grinding to obtain precursor powder;
(2-3) calcining the precursor powder in an electric furnace at 500 ℃ for 30min, removing the coating on SiO2After PEG on the surface layer, the superfine CeO is obtained by grinding2@a-SiO2Coating the precursor powder of a-SiO2Is amorphous SiO2；
(3) gamma-Ce treated with carbon powder2S3@a-SiO2Preparation of
Placing the wrapped precursor powder in an atmosphere furnace, and adding CS2Vulcanizing at the temperature rising rate of 5 ℃/min to 900 ℃ for 120min under the vulcanizing atmosphere formed by the mixed gas of Ar gas to obtain gamma-Ce2S3@a-SiO2(ii) a Then according to the mass ratio of gamma to Ce2S3@a-SiO2Mixing the gamma-Ce powder with carbon powder in the ratio of 1: 12S3@a-SiO2Mixing and grinding with carbon powder to obtain gamma-Ce treated by carbon powder2S3@a-SiO2；
(4) Cristobalite-coated gamma-Ce2S3Preparation of
The gamma-Ce treated by the carbon powder2S3@a-SiO2Placing in an atmosphere furnace, heating to 1300 deg.C at 5 deg.C/min under Ar gas inert gas atmosphereCalcining for 120min to obtain the product gamma-Ce2S3@c-SiO2(c-SiO2Cristobalite), acid washed, calcined at 500 deg.C for 30min in air atmosphere to obtain superfine Na with average particle diameter D50 of 4.02 μm (see figure 1) and cristobalite as inclusion+Ion-doped encapsulated red pigment.
Example two:
this example is PEG, carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) preparation of the stock solution
Cerium source solution: according to the molar ratio Ce3+∶H+∶Urea∶Ba2+3: 2: 8: 0.1, adding Ce (NO)3)3· 6H2O, nitric acid, urea, Ba (NO)3)2Dissolving in mixed solution of ethanol and water in the volume ratio of 1: 1, and mixing to obtain Ba2+An ion-doped cerium source solution;
silicon source solution: tetraethyl orthosilicate and PEG are dissolved in absolute ethyl alcohol according to the mass ratio of 1: 6: 1.6 to obtain a silicon source solution;
(2)CeO2@a-SiO2preparation of coated precursor powder
(2-1) according to the molar ratio Si4+∶Ce3+Pouring the silicon source solution into the cerium source solution, stirring and mixing uniformly, adding nitric acid to adjust the pH value to 2.5, and stirring for 90min under a magnetic stirrer with the rotation speed of 250r/min to obtain a precursor solution;
(2-2) carrying out acid catalysis treatment on the precursor solution in an oven at 55 ℃ for 18h to form transparent acid catalysis gel, then putting the acid catalysis gel into the oven to react at 80 ℃ for 72h to hydrolyze urea to obtain white base catalysis gel, further drying at 80 ℃ and then grinding to obtain precursor powder;
(2-3) calcining the precursor powder in an electric furnace at 600 ℃ for 30min, and removing the coating on SiO2After PEG on the surface layer, the superfine CeO is obtained by grinding2@a-SiO2Before packagingBulk powder of a-SiO2Is amorphous SiO2；
(3) gamma-Ce treated with carbon powder2S3@a-SiO2Preparation of
Placing the wrapped precursor powder in an atmosphere furnace, and adding CS2Carrying out vulcanization treatment for 120min at the temperature rising rate of 5 ℃/min to 850 ℃ under the vulcanization atmosphere formed by the mixed gas of Ar gas and gamma-Ce to obtain2S3@a-SiO2(ii) a Then according to the mass ratio of gamma to Ce2S3@a-SiO2Mixing the gamma-Ce powder with carbon powder in the ratio of 1: 0.82S3@a-SiO2Mixing and grinding with carbon powder to obtain gamma-Ce treated by carbon powder2S3@a-SiO2；
(4) Cristobalite-coated gamma-Ce2S3Preparation of
The gamma-Ce treated by the carbon powder2S3@a-SiO2Placing in an atmosphere furnace, calcining for 60min at the temperature rising rate of 5 ℃/min to 1300 ℃ under the atmosphere of Ar gas inert gas, wherein the calcined product is gamma-Ce2S3@c-SiO2(c-SiO2Cristobalite) is adopted, acid washing is carried out, then calcination is carried out for 60min at 400 ℃ in air atmosphere, and superfine Ba with the average grain diameter D50 of 3.98 mu m and the cristobalite as inclusion is obtained2+Ion-doped encapsulated red pigment.
Example three:
this example is PEG, carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) preparation of the stock solution
Cerium source solution: according to the molar ratio Ce3+∶H+∶Urea∶Li+Adding Ce (NO) at ratio of 4: 2.5: 7: 0.23)3· 6H2O, nitric acid, urea, LiNO3Dissolving in the mixture of alcohol and water in the volume ratio of 2 to 1, and mixing to obtain Li+An ion-doped cerium source solution;
silicon source solution: tetraethyl orthosilicate and PEG are dissolved in absolute ethyl alcohol according to the mass ratio of 1: 7: 1.8 to obtain a silicon source solution;
(2)CeO2@a-SiO2preparation of coated precursor powder
(2-1) according to the molar ratio Si4+∶Ce3+Pouring the silicon source solution into the cerium source solution, stirring and mixing uniformly, adding nitric acid to adjust the pH value to 2.3, and stirring for 120min under a magnetic stirrer with the rotation speed of 400r/min to obtain a precursor solution;
(2-2) carrying out acid catalysis treatment on the precursor solution in an oven at 55 ℃ for 30h to form transparent acid catalysis gel, then putting the acid catalysis gel into the oven to react at 80 ℃ for 96h to hydrolyze urea to obtain white base catalysis gel, further drying at 80 ℃ and then grinding to obtain precursor powder;
(2-3) calcining the precursor powder in an electric furnace at 550 ℃ for 40min, and removing the coating on SiO2After PEG on the surface layer, the superfine CeO is obtained by grinding2@a-SiO2Coating the precursor powder of a-SiO2Is amorphous SiO2；
(3) gamma-Ce treated with carbon powder2S3@a-SiO2Preparation of
According to mass ratio of CeO2@a-SiO2Mixing with carbon powder at ratio of 1: 0.9, adding CeO2@a-SiO2Mixing and grinding the wrapped precursor powder and carbon powder, calcining at 800 ℃ for 60min, placing in an atmosphere furnace, and adding CS2Under the sulfuration atmosphere formed by the mixed gas of Ar gas and the carbon powder, the temperature is raised to 950 ℃ at the rate of 5 ℃/min for sulfuration treatment for 120min to obtain the gamma-Ce treated by the carbon powder2S3@a-SiO2；
(4) Cristobalite-coated gamma-Ce2S3Preparation of
The gamma-Ce treated by the carbon powder2S3@a-SiO2Placing in an atmosphere furnace, calcining for 60min at the temperature rising rate of 5 ℃/min to 1350 ℃ in the atmosphere of Ar gas inert gas, wherein the calcined product is gamma-Ce2S3@c-SiO2(c-SiO2Cristobalite), acid-washed, and thenCalcining at 450 deg.C for 60min in air atmosphere to obtain superfine Li with average particle diameter D50 of 4.56 μm and cristobalite as inclusion+Ion-doped encapsulated red pigment.
Cristobalite coated gamma-Ce prepared in each embodiment of the invention2S3Red coloring material, as shown in FIG. 2, gamma-Ce2S3The colorant is encapsulated in the matrix (see fig. 2 a); the spacing of the lattice fringes indicates that the surface-coating matrix material is cristobalite (see fig. 2 b). The colorimetric values of the coating colors at room temperature are shown in Table 1.
TABLE 1 chroma values at room temperature for the colorants prepared in the examples of the invention
| Examples | L* | a* | b* |
| Example one | 40.24 | 37.31 | 32.02 |
| Example two | 39.76 | 35.42 | 29.80 |
| EXAMPLE III | 39.11 | 36.93 | 30.91 |
The results of FIG. 1 and Table 1 show that the cristobalite-coated gamma-Ce prepared by PEG and carbon powder mixing and refining in the embodiment of the invention2S3The wrapping effect and the high-temperature oxidation resistance of the red pigment are greatly improved, the particle size of the pigment is greatly reduced, the dispersibility is improved, the application field of the red pigment can be effectively widened, and the development of the high-temperature ceramic pigment technology and application is facilitated.
Claims (5)
1. PEG (polyethylene glycol) and carbon powder refined cristobalite coated gamma-Ce2S3The preparation method of the red pigment is characterized by comprising the following steps:
(1) preparation of the stock solution
Cerium source solution: according to the molar ratio Ce3+∶H+Urea and alkali metal ions in a ratio of 1-4: 2-5: 6-12: 0.05-0.8, dissolving soluble cerium salt, acid, Urea and an alkali metal ion source in an alcohol-water mixed solution, and uniformly mixing to obtain a cerium source solution;
silicon source solution: dissolving tetraethyl orthosilicate and PEG (polyethylene glycol) in absolute ethyl alcohol according to the mass ratio of tetraethyl orthosilicate to absolute ethyl alcohol to PEG with the polymerization degree of 600-20000 being 1: 3-10: 0.6-3 to obtain a silicon source solution;
(2) CeO2@a-SiO2preparation of coated precursor powder
(2-1) according to the molar ratio Si4+∶Ce3+Pouring the silicon source solution into a cerium source solution, stirring and mixing uniformly, and adding acid to adjust to obtain a precursor solution with a pH value of 2-3, wherein the ratio of silicon source solution to cerium source solution is 5-15: 1-3; wherein the PEG is used as a cross-linking agent to hydrolyze the tetraethyl orthosilicate to produce SiO2Form a cross-linking effect to control SiO2Particle size of (2) prevents the formation of large SiO in the polycondensation process of the hydrolysis product2An aggregate;
(2-2) carrying out acid catalysis treatment on the precursor solution to form transparent acid catalysis gel, then carrying out heating treatment to form white base catalysis gel, drying and grinding to obtain precursor powder;
(2-3) calcining the precursor powder at the temperature of 150-1000 ℃ for 1-100 min to remove the coating on SiO2The surface layer is crosslinked with PEG among CeO2@ a-SiO2 particles, and then the superfine CeO is obtained by grinding2@a-SiO2Coating the precursor powder of a-SiO2Is amorphous SiO2；
(3) Gamma-Ce treated with carbon powder2S3@a-SiO2Preparation of
According to mass ratio of CeO2@a-SiO21: 0.05-2 of carbon powder, and mixing the CeO2@a-SiO2Mixing and grinding the wrapped precursor powder and carbon powder, calcining at the temperature of 600-800 ℃ for 60-120 min, and then carrying out vulcanization treatment in the atmosphere of inert vulcanization gas to obtain gamma-Ce treated by carbon powder2S3@a-SiO2；
Or, the CeO is added2@a-SiO2Carrying out vulcanization treatment on the wrapped precursor powder in an inert vulcanization gas atmosphere to obtain gamma-Ce2S3@a-SiO2Then according to the mass ratio of gamma to Ce2S3@a-SiO21: 0.05-2 of carbon powder, and mixing the gamma-Ce2S3@a-SiO2Mixing and grinding with carbon powder to obtain the gamma-Ce treated by the carbon powder2S3@a-SiO2；
(4) Cristobalite-coated gamma-Ce2S3Preparation of
Treating the gamma-Ce treated with the carbon powder2S3@a-SiO2Calcining for 60-180 min at 1250-1400 ℃ in an inert gas atmosphere, wherein carbon powder is used as a spatial resistance agent to prevent agglomeration of the wrapping pigment during high-temperature calcination; calcining the calcined product for 30-100 min at 400-700 ℃ in air atmosphere after acid washing to obtain the superfine gamma-Ce powder with the average particle size of 3.8-4.6 mu m2S3@c-SiO2A coated red pigment of c-SiO2Is cristobalite.
2. PEG, carbon according to claim 1Powder-refined cristobalite-coated gamma-Ce2S3The preparation method of the red pigment is characterized by comprising the following steps: carrying out acid catalysis treatment at the temperature of 50-60 ℃ for 12-24 h in the step (2-2); and treating the transparent acid catalysis gel at the temperature of 80-100 ℃ for 48-72 h to form white alkali catalysis gel.
3. The PEG-carbon powder refined cristobalite-coated gamma-Ce as claimed in claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: the temperature of the vulcanization treatment in the step (3) is 800-1100 ℃, and the vulcanization time is 60-180 min.
4. Cristobalite-coated gamma-Ce refined by PEG and carbon powder according to any one of claims 1 to 32S3The product prepared by the preparation method of the red pigment is characterized in that: comprises a cristobalite substrate and gamma-Ce coated in the substrate2S3The colorant particles.
5. The product of claim 4, wherein: the color material has a chroma value ofL *＝35.43～40.54、a *＝32.86～37.54、b *23.90-32.84; calcining at 500-900 ℃ in air atmosphere to obtain red color with chromatic valueL *＝33.14～42.53、a *＝28.56～37.31、b *＝23.94～32.48。
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