CN114084898A - High-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method - Google Patents
High-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant non-agglomerated ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the steps of firstly, uniformly mixing cerium salt, a complex and composite doped ions under the condition of liquid phase to form a precursor solution, drying to form gel, and then forming nano precursor powder by adopting a low-temperature self-propagating combustion method; and then under the vacuum condition, the CS is synthesized in situ in the temperature rise process after the nano-scale carbon powder and the sublimed sulfur are mixed2The gas is taken as a sulfur source to carry out vulcanization treatment, and the superfine gamma-Ce which is high temperature resistant and does not agglomerate is prepared2S3A red colorant. In addition, the product prepared by the preparation method is also disclosed. The invention effectively improves the gamma-Ce2S3High temperature of Red pigmentOn the premise of stability, the granularity of the pigment is reduced, the tinting strength of the pigment is improved, and thus the gamma-Ce is expanded2S3Application field of red pigment.
Description
Technical Field
The invention relates to the technical field of inorganic pigments, in particular to 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 cadmium-selenium red pigment containing heavy metal, and is widely used in the fields of plastic production, printing ink, vehicle paint and the like. However, it is difficult to obtain pure phase γ -Ce at a lower temperature due to the high temperature and many intermediate phases required for its preparation2S3. And gamma-Ce obtained2S3It is decomposed at 350 deg.C in air, and if it is placed in a humid or slightly acidic environment at normal temperature, it is decomposed spontaneously by absorbing moisture.
Currently, researchers use ion doping, for example, by introducing Ba2+、Sr2+、Sm3+、Y3+The composite doping of plasma realizes the reduction of gamma-Ce2S3The temperature of synthesis of (a), but the complex doping is mostly realized by matching divalent alkaline earth metal ions with trivalent rare earth metal ions. And for B3+、P5+Non-metal ions and Na which are not easy to precipitate+、K+And the traditional solid phase method is still adopted for the composite doping of alkali metal ions which are not easy to precipitate. The grinding and doping of the solid phase method cannot achieve atomic level combination, and agglomeration is inevitable in the process of vulcanization and calcination, so that the doping effect is reduced, the prepared pigment particles are large, and the dispersibility is poor. Moreover, the improvement of the stability by the divalent alkaline earth metal ions and the trivalent rare earth metal ions is limited, and the color can not be kept unchanged by calcining for a long time at the temperature of more than 400 ℃. Although the prior art also adopts the method that the surface of the pigment is coated with a layer of colorless transparent and chemically stableHigh-temperature-resistant SiO with good qualitative performance2、ZrO2Or ZrSiO4The film method improves the thermal stability of the pigment after being wrapped, but also can generate particle agglomeration to further cause particle size increase and chromaticity reduction, thereby limiting the gamma-Ce2S3The use of (1).
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The preparation method of the red pigment can effectively improve the gamma-Ce2S3The high temperature stability of the red pigment is realized, the granularity of the pigment is reduced, the tinting strength of the pigment is improved, and thus the gamma-Ce is expanded2S3Application field of red pigment. The invention also aims to provide a product prepared by the preparation method.
The purpose of the invention is realized by the following technical scheme:
the invention provides high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) according to the molar ratio Ce3+0.8-1.3: 0.8-1.6: 0.05-0.5: 0.05-1.8, and Ce (NO)3)3·6H2Dissolving O, a complex, a doping ion a source and a doping ion b source in a solvent capable of being evaporated by heating, adding nitric acid, and uniformly stirring to obtain a precursor solution; the doping ion a is Li+、Na+、K+、Ba2+、Sr2+、Ca2 +、Y3+、Sm3+The doping ion B is B3+；
(2) Standing the precursor solution, heating and drying to evaporate the solvent to form viscous gel;
(3) igniting the gel to obtain fluffy precursor powder with the average particle size of 0.1-0.8 microns;
(4) placing the precursor powder in an atmosphere furnace, pumping the pressure in the furnace to-0.1 MPa, heating to 950-1100 ℃ at the speed of 3-8 ℃/min, and using carbonCS synthesized in situ in the temperature rising process after mixing powder and sublimed sulfur2Taking gas as a sulfur source, preserving heat for 2-5 h for vulcanization treatment, wherein the gas pressure follows CS2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished, keeping the pressure in the furnace at-0.1 MPa, and cooling to room temperature to obtain the alpha and b ion codoped high temperature resistant non-agglomerated ultrafine gamma-Ce2S3A red colorant.
Further, in step (1) of the present invention, nitric acid is an oxidizing agent, and a complex is a reducing agent, and the amount of nitric acid is calculated according to the following thermochemical theory: the ratio of the oxidant multiplied by the total oxidation valence to the reductant multiplied by the total reduction valence is 1: 0.5-1.5.
In the above scheme, the Li in the doped ion a source of the invention+The source is lithium nitrate, lithium oxide, lithium carbonate, lithium hydroxide, lithium hydride, Na+The source is sodium chloride, sodium nitrate, sodium carbonate, K+The source is potassium nitrate, potassium chloride, potassium carbonate, Ba2+The source is barium oxide, barium nitrate, barium carbonate, barium acetate, barium chlorate, barium chloride, barium peroxide, Sr2+The source is strontium carbonate, strontium oxide, strontium nitrate, strontium nitride, strontium hydride, strontium peroxide, Ca2+The source is calcium oxide, calcium hydride, calcium peroxide, calcium chloride, calcium fluoride, calcium carbonate, calcium hydroxide, calcium hypochlorite, Y3+The source is yttrium oxide, yttrium fluoride, yttrium chloride, yttrium nitrate, Sm3+The source is samarium oxide, samarium nitrate, samarium fluoride, samarium chloride and samarium monosulfide; b in the doped ion B source3+The source is boric acid, borax, sodium borate, boric anhydride. The complex is EDTA and citric acid; the solvent is deionized water or absolute ethyl alcohol.
Further, the step (2) is heated and dried at the temperature of 80-160 ℃, and the drying time is 7-15 h. And (4) igniting the gel at the temperature of 300-900 ℃ in the step (3). In the step (4), carbon powder, sublimed sulfur and Ce are mixed according to the molar ratio3+1: 6-12: 0.1-0.6; the average particle size of the carbon powder is 0.2-1.0 micron.
The high-temperature resistant non-agglomerated ultrafine gamma-Ce is utilized2S3Preparation method of red pigmentThe obtained product is prepared from monodisperse gamma-Ce with the average particle size of 3-6 microns2S3The colorant particles. The color material has a chroma value of 25.12-34.52, a-41.85-51.69, and b-24.44-43.65, and has a thermal stability of 600-710 ℃.
The invention has the following beneficial effects:
(1) the invention firstly compositely dopes Li under the liquid phase condition+、Na+、K+、Ba2+、Sr2+、Ca2+、Y3+、Sm3+(doping ion a) and metal ion B3+(doping ion b), because the liquid phase method is used for preparation, the raw materials are uniformly mixed, the obtained precursor solution is dried to form gel, the fluffy nano-scale precursor powder obtained by the low-temperature self-propagating combustion method can also be used for preventing the powder from agglomerating and sintering in the vulcanization process by utilizing the space effect, and therefore the ultrafine powder with the average particle diameter of 3-6 microns is obtained. Compared with the doping of divalent alkaline earth metal ions and trivalent rare earth metal ions in the prior art, the composite doping of the application is realized by B3+The gap filling of the ions, alkali metal ions, alkaline earth metal ions and trivalent rare earth metal ions increases the gamma-Ce2S3Dislocation resistance of the crystal, and because of B3+Easily form metal boron oxide with metal ions, excessive B3 +Will form CeBO3Film coated gamma-Ce2S3The pigment improves the chromaticity and the gamma-Ce2S3The high-temperature stability of the pigment can ensure that the pigment can still keep red at about 700 ℃, and the gamma-Ce is widened2S3The application field of the pigment is beneficial to industrial application.
(2) The invention can use different solvents and different complexes to prepare precursors in the liquid phase preparation method. When absolute ethyl alcohol is used as a solvent and citric acid is used as a complex, the high-temperature-resistant superfine bright red pigment with a > 50 is obtained through a higher volatilization rate and a lower combustion temperature; when deionized water is used as a solvent and EDTA is used as a complex, the superfine and high-temperature-resistant scarlet pigment is also obtained through a slower volatilization rate and a higher combustion temperature.
(3) After the nano-scale carbon powder and the sublimed sulfur are mixed, the CS can be formed in situ at 950-1100 DEG C2The gas is used as a sulfur source, the optimal vulcanization temperature of the precursor powder is 950-1100 ℃, and the too low temperature can cause that the formation of gamma-Ce cannot be finished2S3The chroma of the pigment is affected by the over-high temperature.
(4) The invention has simple preparation process, low requirement on equipment, wide application range of products and easy popularization to the preparation of other pigments. In addition, the invention not only improves the product quality of the finished pigment, but also can well respond to the development trend of the construction and clean production of the national environment-friendly society, and is beneficial to the gamma-Ce2S3Development and popularization of pigment production technology.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows the high temperature resistant, non-agglomerated ultra-fine γ -Ce obtained in the first embodiment of the present invention2S3Particle size distribution of red pigment;
FIG. 2 shows the high temperature resistant non-agglomerated ultra-fine γ -Ce obtained in the first embodiment of the present invention2S3Thermogravimetry-differential thermogram of red colorant.
Detailed Description
The first embodiment is as follows:
this example is a high temperature resistant, non-agglomerating ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) according to the molar ratio Ce3+∶EDTA∶Na+∶B3+1: 1.2: 0.3: 1.2, adding Ce (NO)3)3·6H2O, Ethylene Diamine Tetraacetic Acid (EDTA), NaNO3、H3BO3Dissolving in deionized water, and adding HNO3Adding nitric acid into (oxidant) × 5 (total oxidation number): (EDTA) (reducing agent) × 40 (total reduction number) ═ 1: 0.5, and uniformly stirring by magnetic force to obtain a precursor solution;
(2) putting the precursor solution into an oven at 80 ℃ for heating and drying for 12h, and evaporating water to form viscous gel;
(3) igniting the gel in an electric furnace at 700 ℃, and then preserving heat for 30min to obtain fluffy nano-scale precursor powder with the average particle size of 0.54 micron;
(4) nano carbon powder with average grain size of 0.3 micron and sublimed sulfur are mixed in the molar ratio of carbon powder to sublimed sulfur to Ce3+Mixing at ratio of 1: 8: 0.2, placing into crucible, placing beside the nanometer precursor powder, placing into atmosphere furnace, pumping furnace pressure to-0.1 MPa, heating from room temperature to 1000 deg.C at 5 deg.C/min under vacuum environment, maintaining for 3 hr, and vulcanizing under the action of CS gas pressure2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished to keep the pressure in the furnace at-0.1 MPa, and cooling to room temperature to obtain the Na+、B3+Ion-codoped high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The red colorant, having an average particle size D50 of 4.493 microns (see fig. 1), was resistant to heat up to 702.5 ℃ (see fig. 2).
Example two:
this example is a high temperature resistant, non-agglomerating ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) according to the molar ratio Ce3+Citric acid and Na+∶B3+1: 1.2: 0.3: 1.2, adding Ce (NO)3)3·6H2O, citric acid, NaNO3、H3BO3Dissolving in anhydrous ethanol, and adding HNO3Adding nitric acid into (oxidant) × 5 (total oxidation number): (citric acid (reducing agent) × 40 (total reduction number) ═ 1: 0.6, and magnetically stirring uniformly to obtain a precursor solution;
(2) putting the precursor solution into an oven at 80 ℃ for heating and drying for 12h, and evaporating absolute ethyl alcohol to form viscous gel;
(3) igniting the gel in an electric furnace at 500 ℃, and then preserving heat for 30min to obtain fluffy nano-scale precursor powder with the average particle size of 0.46 micron;
(4) nano-scale carbon powder with the average particle size of 0.3 micron and sublimed sulfur are mixed according to the molar ratio of the carbon powder to the sublimed sulfurSublimed sulfur to Ce3+Mixing at ratio of 1: 8: 0.2, placing into crucible, placing beside the nanometer precursor powder, placing into an atmosphere furnace, pumping the pressure in the furnace to-0.1 MPa, heating to 950 deg.C at 5 deg.C/min under vacuum environment, maintaining the temperature for 3h, and vulcanizing under the action of CS2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished to keep the pressure in the furnace at-0.1 MPa, and cooling to room temperature to obtain the Na+、B3+Ion-codoped high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The red pigment, with an average particle size D50 of 5.374 microns, withstands heat up to 670 ℃.
Example three:
this example is a high temperature resistant, non-agglomerating ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) according to the molar ratio Ce3+∶EDTA∶K+∶B3+1: 1.2: 0.3: 1.2, adding Ce (NO)3)3·6H2O, ethylenediaminetetraacetic acid (EDTA), KNO3、H3BO3Dissolving in deionized water, and adding HNO3Adding nitric acid into (oxidant) × 5 (total oxidation number): (EDTA) (reducing agent) × 40 (total reduction number) ═ 1: 0.6, and uniformly stirring by magnetic force to obtain a precursor solution;
(2) putting the precursor solution into an oven at 80 ℃ for heating and drying for 12h, and evaporating absolute ethyl alcohol to form viscous gel;
(3) igniting the gel in an electric furnace at 700 ℃, and then preserving heat for 30min to obtain fluffy nano-scale precursor powder with the average particle size of 0.51 micron;
(4) nano carbon powder with average grain size of 0.3 micron and sublimed sulfur are mixed in the molar ratio of carbon powder to sublimed sulfur to Ce3+Mixing at ratio of 1: 8: 0.2, placing into crucible, placing beside the nanometer precursor powder, placing into an atmosphere furnace, pumping the pressure in the furnace to-0.1 MPa, heating to 980 deg.C at 5 deg.C/min under vacuum, maintaining the temperature for 3 hr, and vulcanizing under the action of CS2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished to ensure that the furnace is heatedMaintaining internal gas pressure at-0.1 MPa, and cooling to room temperature to obtain K+、B3+Ion-codoped high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The red pigment, with an average particle size D50 of 4.935 microns, withstands heat up to 680 ℃.
Example four:
this example is a high temperature resistant, non-agglomerating ultrafine gamma-Ce2S3The preparation method of the red pigment comprises the following steps:
(1) according to the molar ratio Ce3+∶EDTA∶Ba2+∶B3+1: 1.2: 0.15: 1.2, adding Ce (NO)3)3·6H2O, Ethylene Diamine Tetraacetic Acid (EDTA), Ba (NO)3)2、H3BO3Dissolving in deionized water, and adding HNO3Adding nitric acid into (oxidant) × 5 (total oxidation number): (EDTA) (reducing agent) × 40 (total reduction number) ═ 1: 0.5, and uniformly stirring by magnetic force to obtain a precursor solution;
(2) putting the precursor solution into an oven at 80 ℃ for heating and drying for 12h, and evaporating absolute ethyl alcohol to form viscous gel;
(3) igniting the gel in an electric furnace at 700 ℃, and then preserving heat for 30min to obtain fluffy nano-scale precursor powder with the average particle size of 0.49 micron;
(4) nano carbon powder with average grain size of 0.5 micron and sublimed sulfur are mixed in the molar ratio of carbon powder to sublimed sulfur to Ce3+Mixing at ratio of 1: 10: 0.5, placing into crucible, placing beside the nanometer precursor powder, placing into an atmosphere furnace, pumping the pressure in the furnace to-0.1 MPa, heating from room temperature to 1000 deg.C at 5 deg.C/min under vacuum environment, maintaining for 3 hr, and vulcanizing under the action of CS2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished to keep the pressure in the furnace at-0.1 MPa, and cooling to room temperature to obtain the Ba2+、B3+Ion-codoped high-temperature-resistant non-agglomerated ultrafine gamma-Ce2S3The red pigment, with an average particle size D50 of 5.327 microns, withstands heat up to 685 ℃.
The color values at room temperature of the colorants prepared in the examples of the present invention 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 | 26.31 | 46.37 | 25.84 |
| Example two | 33.65 | 51.26 | 42.03 |
| EXAMPLE III | 31.79 | 47.43 | 35.37 |
| Example four | 30.48 | 47.02 | 34.86 |
Claims (9)
1. High temperature resistant and non-agglomerationUltra-fine gamma-Ce2S3The preparation method of the red pigment is characterized by comprising the following steps:
(1) according to the molar ratio Ce3+0.8-1.3: 0.8-1.6: 0.05-0.5: 0.05-1.8, and Ce (NO)3)3·6H2Dissolving O, a complex, a doping ion a source and a doping ion b source in a solvent capable of being evaporated by heating, adding nitric acid, and uniformly stirring to obtain a precursor solution; the doping ion a is Li+、Na+、K+、Ba2+、Sr2+、Ca2+、Y3 +、Sm3+The doping ion B is B3+；
(2) Standing the precursor solution, heating and drying to evaporate the solvent to form viscous gel;
(3) igniting the gel to obtain fluffy precursor powder with the average particle size of 0.1-0.8 microns;
(4) the precursor powder is placed in an atmosphere furnace, the pressure in the furnace is pumped to-0.1 MPa, the temperature is raised to 950-1100 ℃ at the speed of 3-8 ℃/min, and the CS synthesized in situ in the temperature raising process is obtained after carbon powder and sublimed sulfur are mixed2Taking gas as a sulfur source, preserving heat for 2-5 h for vulcanization treatment, wherein the gas pressure follows CS2Gradually rises to the room pressure; immediately pumping out the gas in the furnace after the vulcanization is finished, keeping the pressure in the furnace at-0.1 MPa, and cooling to room temperature to obtain the alpha and b ion codoped high temperature resistant non-agglomerated ultrafine gamma-Ce2S3A red colorant.
2. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: in the step (1), nitric acid is used as an oxidant, a complex is used as a reducing agent, and the dosage of the nitric acid is calculated according to the following thermochemical theory: the ratio of the oxidant multiplied by the total oxidation valence to the reductant multiplied by the total reduction valence is 1: 0.5-1.5.
3. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: li in the doped ion a source+The source is lithium nitrate, lithium oxide, lithium carbonate, lithium hydroxide, lithium hydride, Na+The source is sodium chloride, sodium nitrate, sodium carbonate, K+The source is potassium nitrate, potassium chloride, potassium carbonate, Ba2+The source is barium oxide, barium nitrate, barium carbonate, barium acetate, barium chlorate, barium chloride, barium peroxide, Sr2+The source is strontium carbonate, strontium oxide, strontium nitrate, strontium nitride, strontium hydride, strontium peroxide, Ca2+The source is calcium oxide, calcium hydride, calcium peroxide, calcium chloride, calcium fluoride, calcium carbonate, calcium hydroxide, calcium hypochlorite, Y3+The source is yttrium oxide, yttrium fluoride, yttrium chloride, yttrium nitrate, Sm3+The source is samarium oxide, samarium nitrate, samarium fluoride, samarium chloride and samarium monosulfide; b in the doped ion B source3+The source is boric acid, borax, sodium borate, boric anhydride.
4. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: the complex is EDTA and citric acid; the solvent is deionized water or absolute ethyl alcohol.
5. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: and (3) heating and drying at the temperature of 80-160 ℃ in the step (2), wherein the drying time is 7-15 h.
6. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: and (4) igniting the gel at the temperature of 300-900 ℃ in the step (3).
7. The high temperature resistant, non-agglomerating ultrafine gamma-Ce of claim 12S3The preparation method of the red pigment is characterized by comprising the following steps: in the step (4), carbon powder, sublimed sulfur and Ce are mixed according to the molar ratio3+＝1∶6～12∶0.1～0.6；The average particle size of the carbon powder is 0.2-1.0 micron.
8. Use of the high temperature resistant, non-agglomerated ultra-fine γ -Ce of any of claims 1-72S3The product prepared by the preparation method of the red pigment is characterized in that: the monodisperse gamma-Ce with the average grain diameter of 3-6 microns2S3The colorant particles.
9. The product of claim 8, wherein: the color material has a chroma value of 25.12-34.52, a-41.85-51.69, and b-24.44-43.65, and has a thermal stability of 600-710 ℃.
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