CN103449518A - Lanthanum, yttrium and cerium co-doped bismuth vanadate inorganic pigment and preparation method thereof - Google Patents
Lanthanum, yttrium and cerium co-doped bismuth vanadate inorganic pigment and preparation method thereof Download PDFInfo
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- CN103449518A CN103449518A CN2013103436747A CN201310343674A CN103449518A CN 103449518 A CN103449518 A CN 103449518A CN 2013103436747 A CN2013103436747 A CN 2013103436747A CN 201310343674 A CN201310343674 A CN 201310343674A CN 103449518 A CN103449518 A CN 103449518A
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Abstract
The invention discloses a lanthanum, yttrium and cerium co-doped bismuth vanadate inorganic pigment and a preparation method thereof. The general formula of the inorganic pigment is Bi1-x-y-zLaxYyCezVO4, wherein x is not less than 0.02 and not more than 0.1, y is not less than 0.02 and not more than 0.1, and z is not less than 0.02 and not more than 0.1; chelating agents are utilized for assistance, and a microwave hydrothermal method is used for preparing the lanthanum, yttrium and cerium co-doped bismuth vanadate pigment; the different chelating agents are added so as to be favorable for slow release of metal ions in a reaction process, thereby enabling the generation process of the lanthanum, yttrium and cerium co-doped bismuth vanadate pigment to proceed more mildly; the microwave hydrothermal method is used to shorten the preparation time; and the doping of the prepared lanthanum element, yttrium element and cerium element is favorable for improving the color-forming performance of the bismuth vanadate pigment.
Description
Technical field
The present invention relates to the mineral dye preparation field, be specifically related to a kind of lanthanum, yttrium and cerium codoped pucherite mineral dye and preparation method thereof.
Background technology
Since the eighties in last century, because pucherite has nontoxic, the high-performances such as color and luster bright, good corrosion resistance, photochemical catalysis, photocatalytic degradation and the large field of mineral dye two have been widely used in.As a kind of environmentally friendly inorganic materials, having replaced gradually environmentally harmful pigment in the pigment field becomes a kind of novel pigment be widely used.In decades recently, scholars to pucherite the application in mineral dye carried out a large amount of research, for example: prepare bismuth vanadium pigments with diverse ways, its main method has: the metal organic decomposition method of solid phase method, pickling process, hydrothermal method, photoreduction method, modification etc.Prepare bismuth vanadium pigments with different raw materials, the raw material of mainly using has Bismuth trinitrate, ammonium meta-vanadate and sodium metavanadate.Also have and in preparing the process of bismuth vanadium pigments, add the different surfaces promoting agent to carry out modification, the tensio-active agent of mainly using has: ethylenediamine tetraacetic acid (EDTA), PVP, cetyl trimethylammonium bromide etc.
Yet these can not meet the application of single pucherite in practical field far away.
Summary of the invention
The invention provides a kind of lanthanum, yttrium and cerium codoped pucherite mineral dye and preparation method thereof, utilize sequestrant to assist and use microwave-hydrothermal method to prepare the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, lanthanum element, yttrium and Ce elements doped with the color generation property that helps improve bismuth vanadium pigments.
The present invention is by the following technical solutions:
A kind of lanthanum, yttrium and cerium codoped pucherite mineral dye preparation method, utilize sequestrant to assist and use microwave-hydrothermal method to prepare the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped.
Specifically comprise the following steps:
(1), by Bi (NO
3)
35H
2o, La (NO
3)
3, Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o and sequestrant are dissolved into the HNO of 1~4mol/L
3in solution and carry out fully stirring and obtaining solution A, wherein Bi (NO
3)
35H
2o, La (NO
3)
3, Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o, HNO
3with the mol ratio of sequestrant be 1:(0.02~0.1): (0.02~0.1): (0.02~0.1): (4~16): (0.5~2); By NaVO
32H
2o is dissolved in the NaOH solution of 1~4mol/L and carries out fully stirring and obtaining solution B, wherein NaVO
32H
2the mol ratio of O and NaOH is 1:(4~16);
(2), by solution A with solution B is mixed and carry out fully stirring and form suspension, wherein Bi
3+and VO
3-mol ratio be 1:1, the presoma of the bismuth vanadium pigments that this suspension is lanthanum, yttrium and cerium element co-doped;
(3), above-mentioned suspension is transferred in the microwave hydrothermal instrument, utilize carry out microwave radiation heating; After microwave hydrothermal reacts completely, wash several times, make the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped after vacuum-drying.
Described sequestrant is ethylenediamine tetraacetic acid (EDTA), Trisodium Citrate, methyl ethyl diketone or several mixtures.
Step is transferred to suspension in the microwave hydrothermal instrument in (3), utilizes carry out microwave radiation heating will arrive 160 ℃~220 ℃, hydro-thermal reaction 1~3h.
After in step (3), microwave hydrothermal reacts completely, with deionized water and absolute ethanol washing several times.
In step (3) after washing in vacuum drying oven dry 12h under 60 ℃, make the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped.
A kind of lanthanum, yttrium and cerium codoped pucherite mineral dye, its general formula is Bi
1-x-y-zla
xy
yce
zvO
4, 0.02≤x≤0.1,0.02≤y≤0.1,0.02≤z≤0.1 wherein.
Beneficial effect of the present invention is: add different sequestrants, it act as and contributes to the slow release of metal ion in reaction process, thereby the carrying out that the process that makes to generate lanthanum, yttrium and cerium element co-doped bismuth vanadium pigments relatively relaxes, the bismuth vanadium pigments chemical constitution obtained is even, particle diameter is less, and in the certain particle size scope, particle diameter is less, its opacifying power, tinting strength are stronger, from but dominant hue and the brightness of pigment improve; Use microwave-hydrothermal method to prepare the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, its synthesis temperature is lower, generated time is shorter, and the synthetic required synthesis temperature of bismuth vanadium pigments of conventional solid-state method is higher, generated time is longer, therefore, preparation method provided by the present invention is conducive to reduce energy consumption, reduces production costs; The bismuth vanadium pigments that the product that the present invention finally makes is lanthanum, yttrium and cerium element co-doped, utilize lanthanum, yttrium and cerium element doped with the color generation property that helps improve bismuth vanadium pigments, because the atomic structure of rare earth element uniqueness, the existence of the 4f electronic shell be not full of, when being subject to rayed, the have characteristic that selectivity absorb and reflect of 4f electronic shell to light, due to this specific character, can make rare earth doped beramic color have advantages of that color development is stable, tone is pure.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 1mol/L, the HNO of 20ml
3in solution, then add wherein 0.1mmol(0.0325g) La (NO
3)
3, 0.1mmol(0.0383g) Y (NO
3)
36H
2o, 0.1mmol(0.0434g) Ce (NO
3)
36H
2o and 2.5mmol(0.7306g) ethylenediamine tetraacetic acid (EDTA), fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 1mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 160 ℃, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.94la
0.02y
0.02ce
0.02vO
4.
Embodiment 2:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 4mol/L, the HNO of 20ml
3in solution, then add wherein 0.1mmol(0.0325g) La (NO
3)
3, 0.1mmol(0.0383g) Y (NO
3)
36H
2o, 0.1mmol(0.0434g) Ce (NO
3)
36H
2o and 10mmol(2.9224g) ethylenediamine tetraacetic acid (EDTA), fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 4mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 220 ℃, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.94la
0.02y
0.02ce
0.02vO
4.
Embodiment 3:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 1mol/L, the HNO of 20ml
3in solution, then add wherein 0.1mmol(0.0325g) La (NO
3)
3, 0.1mmol(0.0383g) Y (NO
3)
36H
2o, 0.1mmol(0.0434g) Ce (NO
3)
36H
2o and 2.5mmol(0.7353g) Trisodium Citrate, fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 1mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 160 ℃, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.94la
0.02y
0.02ce
0.02vO
4.
Embodiment 4:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 4mol/L, the HNO of 20ml
3in solution, then add wherein 0.5mmol(0.1625g) La (NO
3)
3, 0.5mmol(0.1915g) Y (NO
3)
36H
2o, 0.5mmol(0.217g) Ce (NO
3)
36H
2o and 10mmol(2.9412g) Trisodium Citrate, fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 4mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 220 ℃, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.7la
0.1y
0.1ce
0.1vO
4.
Embodiment 5:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 1mol/L, the HNO of 20ml
3in solution, then add wherein 0.5mmol(0.1625g) La (NO
3)
3, 0.5mmol(0.1915g) Y (NO
3)
36H
2o, 0.5mmol(0.217g) Ce (NO
3)
36H
2o and 2.5mmol(0.2503g) methyl ethyl diketone, fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 1mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 160 ℃, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.7la
0.1y
0.1ce
0.1vO
4.
Embodiment 6:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 4mol/L, the HNO of 20ml
3in solution, then add wherein 0.5mmol(0.1625g) La (NO
3)
3, 0.5mmol(0.1915g) Y (NO
3)
36H
2o, 0.5mmol(0.217g) Ce (NO
3)
36H
2o and 10mmol(1.0012g) methyl ethyl diketone, fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 4mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 220 ℃, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.7la
0.1y
0.1ce
0.1vO
4.
Embodiment 7:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 2.5mol/L, the HNO of 20ml
3in solution, then add wherein 0.3mmol(0.0975g) La (NO
3)
3, Y (NO 0.3mmol(0.1149g)
3)
36H
2o, 0.3mmol(0.1302g) Ce (NO
3)
36H
2o, 8mmol(0.80096g) methyl ethyl diketone and ethylenediamine tetraacetic acid (EDTA), fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 2.5mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 185 ℃, and microwave hydrothermal 2h.Then, with deionized water and absolute ethanol washing several times, dry 12h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.82la
0.06y
0.06ce
0.06vO
4.
Embodiment 8:
By 5mmol(2.4254g) Bi (NO
3)
35H
2o is dissolved into 3mol/L, the HNO of 20ml
3in solution, then add wherein 0.4mmol(0.13216g) La (NO
3)
3, 0.4mmol(0.1532g) Y (NO
3)
36H
2o, 0.4mmol(0.1736g) Ce (NO
3)
36H
2o, 6mmol(0.60072g) the mixture of ethylenediamine tetraacetic acid (EDTA), methyl ethyl diketone and Trisodium Citrate, fully stir to obtain solution A; By 5mmol(0.7898g) NaVO
32H
2o is dissolved into 3mol/L, in the NaOH solution of 20ml, fully stirs to obtain solution B; By above-mentioned A, B solution mixes and fully forwards in water heating kettle after stirring, under 200 ℃, and microwave hydrothermal 2.5h.Then, with deionized water and absolute ethanol washing several times, dry 1.5h under 60 ℃ in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, and its general formula is Bi
0.76la
0.08y
0.08ce
0.08vO
4.
In the present invention, added different sequestrants, can effectively control speed of reaction, made to generate the carrying out of the process gentleness of bismuth vanadium pigments; Secondly, the present invention improves the color generation property of bismuth vanadium pigments by the co-doped of lanthanum, yttrium and cerium element; Finally, the present invention uses the microwave-hydrothermal method that can effectively shorten preparation time to carry out the preparation of bismuth vanadium pigments.
Claims (7)
1. a lanthanum, yttrium and cerium codoped pucherite mineral dye preparation method, is characterized in that: utilize sequestrant to assist and use microwave-hydrothermal method to prepare the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped.
2. lanthanum according to claim 1, yttrium and cerium codoped pucherite mineral dye preparation method, is characterized in that, specifically comprises the following steps:
(1), by Bi (NO
3)
35H
2o, La (NO
3)
3, Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o and sequestrant are dissolved into the HNO of 1~4mol/L
3in solution and carry out fully stirring and obtaining solution A, wherein Bi (NO
3)
35H
2o, La (NO
3)
3, Y (NO
3)
36H
2o, Ce (NO
3)
36H
2o, HNO
3with the mol ratio of sequestrant be 1:(0.02~0.1): (0.02~0.1): (0.02~0.1): (4~16): (0.5~2); By NaVO
32H
2o is dissolved in the NaOH solution of 1~4mol/L and carries out fully stirring and obtaining solution B, wherein NaVO
32H
2the mol ratio of O and NaOH is 1:(4~16);
(2), by solution A with solution B is mixed and carry out fully stirring and form suspension, wherein Bi
3+and VO
3-mol ratio be 1:1, the presoma of the bismuth vanadium pigments that this suspension is lanthanum, yttrium and cerium element co-doped;
(3), above-mentioned suspension is transferred in the microwave hydrothermal instrument, utilize carry out microwave radiation heating; After microwave hydrothermal reacts completely, wash several times, make the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped after vacuum-drying.
3. lanthanum according to claim 1 and 2, yttrium and cerium codoped pucherite mineral dye preparation method, it is characterized in that: described sequestrant is ethylenediamine tetraacetic acid (EDTA), Trisodium Citrate, methyl ethyl diketone or several mixtures.
4. lanthanum according to claim 2, yttrium and cerium codoped pucherite mineral dye preparation method, it is characterized in that: step is transferred to suspension in the microwave hydrothermal instrument in (3), utilizes carry out microwave radiation heating will arrive 160 ℃~220 ℃, hydro-thermal reaction 1~3h.
5. lanthanum according to claim 2, yttrium and cerium codoped pucherite mineral dye preparation method, is characterized in that: after in step (3), microwave hydrothermal reacts completely, with deionized water and absolute ethanol washing several times.
6. lanthanum according to claim 2, yttrium and cerium codoped pucherite mineral dye preparation method is characterized in that: in step (3) after washing in vacuum drying oven dry 12h under 60 ℃, make the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped.
7. lanthanum, yttrium and the cerium codoped pucherite mineral dye made as claim 1-6 preparation method, it is characterized in that: its general formula is Bi
1-x-y-zla
xy
yce
zvO
4, 0.02≤x≤0.1,0.02≤y≤0.1,0.02≤z≤0.1 wherein.
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CN106915762A (en) * | 2017-03-15 | 2017-07-04 | 包头稀土研究院 | Double rare earth oxide materials with nanostructured and preparation method thereof |
CN107286776A (en) * | 2017-07-21 | 2017-10-24 | 南京理工大学 | Infrared-reflection heat-insulation coating based on cerium dopping compound and preparation method thereof |
CN109181369A (en) * | 2018-10-15 | 2019-01-11 | 中国科学院兰州化学物理研究所 | Microwave hydrothermal auxiliary prepares high chroma cobalt blue/clay mineral hybrid pigment method |
CN114477266A (en) * | 2022-02-11 | 2022-05-13 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
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CN106915762A (en) * | 2017-03-15 | 2017-07-04 | 包头稀土研究院 | Double rare earth oxide materials with nanostructured and preparation method thereof |
CN107286776A (en) * | 2017-07-21 | 2017-10-24 | 南京理工大学 | Infrared-reflection heat-insulation coating based on cerium dopping compound and preparation method thereof |
CN107286776B (en) * | 2017-07-21 | 2019-06-25 | 南京理工大学 | Infrared-reflection heat-insulation coating and preparation method thereof based on cerium dopping compound |
CN109181369A (en) * | 2018-10-15 | 2019-01-11 | 中国科学院兰州化学物理研究所 | Microwave hydrothermal auxiliary prepares high chroma cobalt blue/clay mineral hybrid pigment method |
CN114477266A (en) * | 2022-02-11 | 2022-05-13 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
CN114477266B (en) * | 2022-02-11 | 2024-01-23 | 包头稀土研究院 | Method for improving near infrared reflectivity of yellow pigment |
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