CN111057399A - Preparation method of rare earth doped clay mineral-based bismuth yellow hybrid pigment with adjustable fluorescence and color - Google Patents
Preparation method of rare earth doped clay mineral-based bismuth yellow hybrid pigment with adjustable fluorescence and color Download PDFInfo
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Abstract
The invention provides a preparation method of a rare earth-doped clay mineral-based bismuth yellow hybrid pigment with adjustable fluorescence and color, which is characterized in that a rare earth element hydrate salt and a bismuth salt are fully dissolved in a nitric acid solution to form a solution A; stirring, dissolving and dispersing vanadium salt and clay mineral in nitric acid or sodium hydroxide solution to form suspension B; then dropwise adding the solution A into the suspension B, adding a pH regulator to regulate the pH of the mixed solution to 6-8, and stirring for reaction for 0.5-3 h; and centrifugally washing the reaction product to be neutral, calcining and crushing to obtain the rare earth doped clay mineral-based bismuth yellow hybrid pigment. According to the invention, the clay mineral is introduced to realize the regulation and control of the particle size and the particle size distribution of the bismuth yellow hybrid pigment, and the preparation cost of the high-grade bismuth yellow pigment is effectively reduced; the bismuth yellow hybrid pigment prepared by introducing rare earth elements and clay minerals has fluorescence adjustable performance; the rare earth doped clay mineral-based bismuth yellow hybrid pigment is prepared by a chemical precipitation method, and has the advantages of simple and convenient operation and strong controllability.
Description
Technical Field
The invention relates to a preparation method of a rare earth doped clay mineral based bismuth yellow hybrid pigment, in particular to a preparation method of a rare earth doped clay mineral based bismuth yellow hybrid pigment with adjustable fluorescence and color, belonging to the technical field of environment-friendly inorganic pigments.
Background
The yellow light wave range is 565-595 nm, and is in the most sensitive wave band (400-700 nn) of human eyeball to light. Therefore, yellow inorganic pigments, which are high-visibility warning pigments, are widely used in places requiring high eye-catching in traffic, roads, hoisting machinery, and the like. Among the numerous yellow inorganic pigments, bismuth yellow pigment (BiVO)4) The reflectivity at 450 nm is obviously higher than that of other pigments, and the environment-friendly yellow inorganic pigment has excellent performance. However, bismuth yellow pigment is expensive and inevitably causes grain growth and agglomeration during the heat treatment process. Research shows that the agglomeration phenomenon of inorganic nano particles can be obviously improved by introducing the carrier material, and particularly, the agglomeration phenomenon of the inorganic nano pigment is effectively improved and the production cost of the environment-friendly inorganic pigment is greatly reduced by introducing the environment-friendly hybrid inorganic pigment prepared from natural clay minerals.
The rare earth element is active in property, has a unique 4f electronic structure, has a trivalent ion state and an ionic radius of 0.84-1.06 Å, integrates the unique electronic structure, strong spin orbit effect, large atomic magnetic moment and other characteristics of the rare earth vanadate and the nanometer characteristics, and has good application prospect in the fields of ceramics, luminescent materials, catalysts, environment-friendly materials and the like3+The valence state of the rare earth ions is the same as that of the rare earth ions, and the ionic radius is similar, so the rare earth elements are often used as doping elements to prepare rare earth doped bismuth vanadate, and the prepared product has good luminous and photocatalytic hydrogen production performance. BiVO synthesized by Starsich et al4: Nd3+The fluorescent nanoparticles can be observed at the depth of 20 mm, and have good spatial resolution and light stabilityHigh qualitative characteristics (chem. Mater. 2017, 29, 8158-8166). At present, the research of the rare earth doping bismuth vanadate material mainly focuses on the field of photocatalysis, but the influence rule of the rare earth doping on the color of the bismuth vanadate pigment is rarely researched. Sameera et al prepared Li by conventional solid phase reaction0.10RE0.10Bi0.8Mo0.2V0.8O4(RE = La, Pr, Sm, Gd, Tb, Dy, Y, Yb, Lu) high reflectance yellow inorganic pigment, but the effect of the rare earth doping amount on the chromaticity of bismuth yellow pigment was not investigated (ACS Sustainable chem. Eng. 2015, 3, 1227-doped 1233). As is known, there is a certain relationship between the band gap energy of a material and its color, doping with different amounts and different rare earth elements easily causes deformation and distortion of bismuth vanadate crystal lattice, resulting in a change in energy difference (i.e., band gap energy) between the bismuth vanadate conduction band and valence band, and finally realizing the adjustment and control of its chromaticity, which can be potentially applied in the field of luminescent materials.
Disclosure of Invention
The invention aims to provide a method for preparing rare earth-doped clay mineral-based bismuth yellow hybrid pigment by a chemical precipitation method aiming at the defects of the existing bismuth yellow pigment preparation technology and the requirements of color performance, and develops a preparation technology of the bismuth yellow pigment with adjustable fluorescence and color.
Preparation of rare earth doped clay mineral based bismuth yellow hybrid pigment
Fully dissolving rare earth element hydrate salt and bismuth salt in a nitric acid solution (with the concentration of 1-8 mol/L) to form a solution A; stirring, dissolving and dispersing vanadium salt and clay mineral in a nitric acid solution (with the concentration of 1-8 mol/L) or a sodium hydroxide solution (with the concentration of 1-8 mol/L) to form a light yellow suspension B; then dropwise adding the solution A into the suspension B, adding a pH regulator to regulate the pH of the mixed solution to 6-8, and stirring for reaction for 0.5-3 h; and after centrifugally washing the reaction product to be neutral, calcining at 300-800 ℃ for 0.5-4 h, crushing and sieving to obtain the rare earth doped clay mineral-based bismuth yellow hybrid pigment.
The rare earth element hydrated salt is at least one of europium nitrate, gadolinium nitrate, cerium nitrate, samarium nitrate, lanthanum nitrate, europium chloride, gadolinium chloride, cerium chloride, samarium chloride, lanthanum chloride, europium acetate, gadolinium acetate, cerium acetate, samarium acetate and lanthanum acetate. The bismuth source is at least one of bismuth oxide, bismuth nitrate, bismuth chloride, bismuth acetate or bismuth sulfate. The ratio of the rare earth element hydrated salt to the bismuth source is 0.005-0.1: 1.
The vanadium source is at least one of vanadium pentoxide, ammonium metavanadate, sodium metavanadate or sodium vanadate. The ratio of the sum of the amounts of the bismuth source and the dopant substance to the amount of the vanadium source substance is 1:0.5 to 1: 5.
The clay mineral is at least one of attapulgite, kaolin, halloysite, talc, wollastonite, montmorillonite, sepiolite and illite, and the addition amount of the clay mineral is measured by the mass percentage content of the clay mineral in the rare earth doped bismuth yellow pigment being 10-80%.
The pH regulator is at least one of ammonia water, sodium hydroxide, potassium hydroxide, sodium phosphate, sodium monohydrogen phosphate, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
Structure and performance characterization of rare earth doped clay mineral-based bismuth yellow hybrid pigment
1. X-ray diffraction spectrum
FIG. 1 shows the X-ray diffraction pattern of the bismuth yellow pigment prepared by the present invention. As shown in the figure, in2θMonoclinic scheelite-type BiVO appears at = 18.681 °, 18.989 °, 28.921 °, 30.531 °, 34.511 °, 35.201 °, 39.561 °, 39.781 °, 40.050 ° and 42.470 °4Corresponding to the (011), (112), (004), (200), (020), (211), (121) and (015) crystal planes, respectively. The characteristic peaks of the bismuth yellow hybrid pigment without doping the rare earth element and the bismuth yellow pigment without introducing the Clay mineral are shifted (appl. Clay Sci.2019, 181, 105221), which indicates that the rare earth element and the Clay mineral obviously cause the distortion of the crystal lattice of the bismuth yellow pigment, and the distortion is probably caused by the co-doping effect of the rare earth element and the main elements of the Clay mineral in the high-temperature crystallization process.
2. Transmission electron microscopy analysis
FIG. 2 is a diagram of a catalyst prepared according to the present inventionLaTransmission electron microscopy (a, b) and high resolution transmission electron microscopy of doped halloysite-based bismuth yellow hybrid pigmentsPhotograph (c). As shown in the graphs a and b, bismuth vanadate particles are successfully loaded on the wall and the inside of the tubular halloysite pipe; while it is confirmed from the lattice spacing of FIG. 2c that it is a monoclinic scheelite-type BiVO4The (-121) plane of (2).
3. Color properties of bismuth yellow hybrid pigments
CIE-L * a * b * The color parameters are shown in table 1. Of bismuth yellow hybrid pigmentsb * The value ranges from 82.00 to 90.12, anda * the values are below 1 except for the H-4 sample reaching 5.32, and even up to-1.13, especially for the H-3 sample, indicating an enhanced green phase. The brightness of five sample samples was found simultaneouslyL * Are all above 78. The maximum absorption edges of the comparative samples, Kubelka-Munk curves (FIG. 3), from H-1 to H-5, are 497.66nm, 502.00nm, 503.01nm, 507.53nm, and 505.02nm, respectively, and the band gap energy values of the five example samples were calculated to be 2.49eV, 2.47eV, 2.44eV, and 2.46eV, respectively. The doping of the doping elements causes the bismuth vanadate to react according to the correlation between the chromaticity and the band gap energy of the inorganic pigmentBi 6s AndO 2p the hybrid orbitals form an energy difference between the valence and conduction bands, resulting in a change in the chromaticity of bismuth vanadate. The analysis shows that the successful doping of the rare earth elements causes the change of the chromaticity and band gap energy of the clay mineral-based bismuth yellow hybrid pigment, thereby realizing the successful regulation and control of the chromaticity of the bismuth vanadate.
In summary, the method for preparing the bismuth yellow hybrid pigment has the following advantages compared with the prior art and the product:
1. by introducing clay minerals, the particle size and particle size distribution of the bismuth yellow hybrid pigment are regulated and controlled, and the preparation cost of the high-grade bismuth yellow pigment is effectively reduced;
2. by introducing rare earth elements and clay minerals, the prepared bismuth yellow hybrid pigment has fluorescence and color adjustability, and is expected to be used in the fields of highway warning boards, high-grade automobile finish paint and the like;
3. the rare earth doped clay mineral-based bismuth yellow hybrid pigment is prepared by a chemical precipitation method, and has the advantages of simple and convenient operation and strong controllability.
Drawings
FIG. 1 shows the X-ray diffraction pattern of the rare earth-doped clay mineral-based bismuth yellow hybrid pigment prepared by the present invention.
FIG. 2 is a transmission electron micrograph of the bismuth yellow hybrid pigment prepared by the present invention.
FIG. 3 is a Kubelka-munk curve of the bismuth yellow hybrid pigment prepared by the invention.
Detailed Description
The preparation and performance of the rare earth doped clay mineral based bismuth yellow hybrid pigment of the invention are further illustrated by the following specific examples.
Example 1
Dissolving 0.483g of bismuth nitrate and 0.002g of lanthanum nitrate in 5mol/L nitric acid solution to form A solution; dissolving 0.160g of sodium metavanadate in 5mol/L sodium hydroxide solution, adding 0.200g of halloysite, and fully stirring and uniformly dispersing to form a suspension B; then the solution A is dripped into the suspension B, and Na is added2CO3After the pH value is adjusted to 6.5, stirring for 1 hour by magnetic force; the product is centrifugally washed to be neutral and then is placed at 100oC, drying in an oven for 2 hours to obtain a precursor; finally, placing the precursor in a muffle furnace, and calcining for 2h at 700 ℃; grinding, crushing and sieving the product to obtain the lanthanum element doped clay mineral-based bismuth yellow hybrid pigment marked as H-1L * 、a * 、b * The color parameters are shown in table 1.
Example 2
Dissolving 0.284g of bismuth chloride and 0.043g of cerium nitrate in a 2mol/L nitric acid solution to form a solution A; 0.5849g of ammonium metavanadate and 0.259g of talc are added into 2mol/L nitric acid solution, stirred, dissolved and dispersed for 0.5h to form suspension B, then the solution A is dropwise added into the suspension B, sodium phosphate is added to adjust the pH value to 7, and stirring is continued for 3 h; centrifugally washing to be neutral, and directly placing the washed solution in a muffle furnace to calcine the solution for 4 hours at 300 ℃; the product is crushed and sieved to obtain cerium doped talc/bismuth yellow hybrid pigment, the sample is marked as H-2,it is composed ofL * 、a * 、b * The color parameters are shown in table 1.
Example 3
Dissolving 0.352g of bismuth sulfate and 0.0007g of europium acetate in a 2mol/L nitric acid solution to form a solution A; adding 0.092g of sodium vanadate and 0.032g of kaolin into 8mol/L sodium hydroxide solution, stirring, dissolving and dispersing for 2 hours to form suspension B; then dropwise adding the solution A to the suspension B, adding ammonia water to adjust the pH value to 8, and continuously stirring for 1.5 h; the reaction product is directly placed in a muffle furnace to be calcined for 0.5H at 800 ℃ after being centrifugally washed to be neutral, and is crushed and sieved to obtain the europium-doped kaolinite-based bismuth yellow hybrid pigment, wherein the sample is marked as H-3, and the europium-doped kaolinite-based bismuth yellow hybrid pigment is obtainedL * 、a * 、b * The color parameters are shown in table 1.
Example 4
Dissolving 0.387g of bismuth nitrate, 0.046g of bismuth oxide and 0.001g of samarium nitrate in 8mol/L nitric acid solution to form solution A; 0.1117g of ammonium metavanadate and 0.162g of sepiolite are added into a 4mol/L nitric acid solution to be stirred, dissolved and dispersed for 1 hour to form a suspension B; then dropwise adding the solution A into the suspension B, adding sodium hydroxide to adjust the pH value to 7, and continuously stirring for 1 h; the product is centrifugally washed to be neutral, then is directly placed in a muffle furnace to be calcined for 1H at the temperature of 600 ℃, is crushed and sieved to obtain samarium-doped sepiolite/bismuth yellow hybrid pigment, the sample is marked as H-4, and the samarium-doped sepiolite/bismuth yellow hybrid pigment is obtainedL * 、a * 、b * The color parameters are shown in table 1.
Example 5
Dissolving 0.314g of bismuth chloride and 0.002g of gadolinium nitrate in 1mol/L nitric acid solution to form solution A; adding 0.113g of sodium metavanadate, 0.091g of vanadium pentoxide and 0.065g of montmorillonite into 2mol/L nitric acid solution, stirring, dissolving and dispersing to form suspension B; then dropwise adding the solution A to the suspension B, adding ammonia water to adjust the pH value to 6, and continuously stirring for 3 hours; the product is directly placed in a muffle furnace to be calcined for 2 hours at 500 ℃ after being centrifugally washed to be neutral, and is crushed and sieved to obtain the gadolinium element doped montmorillonite/bismuth yellow hybrid pigment, wherein the sample is marked as H-5, and the gadolinium element doped montmorillonite/bismuth yellow hybrid pigment is obtainedL * 、a * 、b * The color parameters are shown in table 1.
Claims (10)
1. A preparation method of a rare earth-doped clay mineral-based bismuth yellow hybrid pigment with adjustable fluorescence and color comprises the steps of fully dissolving a rare earth element hydrate salt and a bismuth salt in a nitric acid solution to form a solution A; stirring, dissolving and dispersing vanadium salt and clay mineral in a nitric acid solution or a sodium hydroxide solution to form a light yellow suspension B; then dropwise adding the solution A into the suspension B, adding a pH regulator to regulate the pH of the mixed solution to 6-8, and stirring for reaction for 0.5-3 h; and after centrifugally washing the reaction product to be neutral, calcining at 300-800 ℃ for 0.5-4 h, crushing and sieving to obtain the rare earth doped clay mineral-based bismuth yellow hybrid pigment.
2. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the rare earth element hydrated salt is at least one of europium nitrate, gadolinium nitrate, cerium nitrate, samarium nitrate, lanthanum nitrate, europium chloride, gadolinium chloride, cerium chloride, samarium chloride, lanthanum chloride, europium acetate, gadolinium acetate, cerium acetate, samarium acetate and lanthanum acetate.
3. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the bismuth source is at least one of bismuth oxide, bismuth nitrate, bismuth chloride, bismuth acetate or bismuth sulfate.
4. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the ratio of the rare earth element hydrated salt to the bismuth source is 0.005-0.1: 1.
5. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the vanadium source is at least one of vanadium pentoxide, ammonium metavanadate, sodium metavanadate or sodium vanadate.
6. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the ratio of the sum of the amounts of the bismuth source and the dopant substance to the amount of the vanadium source substance is 1:0.5 to 1: 5.
7. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the clay mineral is at least one of attapulgite, kaolin, halloysite, talc, wollastonite, montmorillonite, sepiolite and illite, and the addition amount of the clay mineral is measured by the mass percentage content of the clay mineral in the rare earth doped bismuth yellow pigment being 10-80%.
8. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the pH regulator is at least one of ammonia water, sodium hydroxide, potassium hydroxide, sodium phosphate, sodium monohydrogen phosphate, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
9. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the nitric acid solution is 1-8 mol/L.
10. The preparation method of the fluorescence and color tunable rare earth doped clay mineral-based bismuth yellow hybrid pigment as claimed in claim 1, wherein the preparation method comprises the following steps: the concentration of the sodium hydroxide solution is 1-8 mol/L.
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Cited By (3)
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|---|---|---|---|---|
| CN113929141A (en) * | 2021-09-28 | 2022-01-14 | 厦门稀土材料研究所 | High near-infrared reflection rare earth yellow pigment and preparation method and application thereof |
| CN114410127A (en) * | 2022-01-21 | 2022-04-29 | 中国科学院兰州化学物理研究所 | Method for efficiently and cleanly preparing clay mineral hybrid bismuth yellow pigment |
| CN114644839A (en) * | 2022-04-22 | 2022-06-21 | 中国科学院兰州化学物理研究所 | Environment-friendly yellow inorganic pigment with high near-infrared reflectivity and preparation method thereof |
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| CN114410127A (en) * | 2022-01-21 | 2022-04-29 | 中国科学院兰州化学物理研究所 | Method for efficiently and cleanly preparing clay mineral hybrid bismuth yellow pigment |
| CN114644839A (en) * | 2022-04-22 | 2022-06-21 | 中国科学院兰州化学物理研究所 | Environment-friendly yellow inorganic pigment with high near-infrared reflectivity and preparation method thereof |
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