CN103449518B - 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 PDF

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CN103449518B
CN103449518B CN201310343674.7A CN201310343674A CN103449518B CN 103449518 B CN103449518 B CN 103449518B CN 201310343674 A CN201310343674 A CN 201310343674A CN 103449518 B CN103449518 B CN 103449518B
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yttrium
lanthanum
cerium
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CN103449518A (en
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李军奇
张炼
刘辉
何选盟
朱振峰
崔明明
刘振兴
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Zhongshan perfect color resource Co., Ltd.
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Shaanxi University of Science and Technology
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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

A kind of lanthanum, yttrium and cerium codoped pucherite mineral dye and preparation method thereof
Technical field
The present invention relates to 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 the high-performance such as nontoxic, bright color, good corrosion resistance, photochemical catalysis, photocatalytic degradation and the large field of mineral dye two are widely used in.As a kind of environmentally friendly inorganic materials, in pigment art, instead of environmentally harmful pigment gradually becomes a kind of novel pigment be widely used.In nearest decades, scholars have carried out large quantifier elimination to the application of pucherite in mineral dye, such as: prepare bismuth vanadium pigments with diverse ways, its main method has: the metallo-organic chemical vapour deposition etc. of solid phase method, pickling process, hydrothermal method, photoreduction method, modification.Prepare bismuth vanadium pigments with different raw materials, the raw material mainly used has Bismuth trinitrate, ammonium meta-vanadate and sodium metavanadate.Also have and in the process preparing bismuth vanadium pigments, to add different surfaces promoting agent carry out modification, the tensio-active agent mainly used has: ethylenediamine tetraacetic acid (EDTA), PVP, cetyl trimethylammonium bromide etc.
But 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 helping the color generation property improving 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 3carry out fully stirring obtaining solution A, wherein Bi (NO in solution 3) 35H 2o, La (NO 3) 3, Y (NO 3) 36H 2o, Ce (NO 3) 36H 2o, HNO 3be 1:(0.02 ~ 0.1 with the mol ratio of sequestrant): (0.02 ~ 0.1): (0.02 ~ 0.1): (4 ~ 16): (0.5 ~ 2); By NaVO 32H 2o to be dissolved in the NaOH solution of 1 ~ 4mol/L and to carry out fully stirring obtaining solution B, wherein NaVO 32H 2the mol ratio of O and NaOH is 1:(4 ~ 16);
(2), solution A and solution B mixed and carry out fully stirring forming suspension, wherein Bi 3+and VO 3-mol ratio be 1:1, this suspension is the presoma of the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped;
(3), by above-mentioned suspension be transferred in microwave hydrothermal instrument, utilize carry out microwave radiation heating; After microwave hydrothermal reacts completely, washing several times, the bismuth vanadium pigments of obtained 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.
Suspension is transferred in microwave hydrothermal instrument in (3) by step, utilizes carry out microwave radiation heating will to 160 DEG C ~ 220 DEG C, 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 at 60 DEG C, the bismuth vanadium pigments of obtained 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, wherein 0.02≤x≤0.1,0.02≤y≤0.1,0.02≤z≤0.1.
Beneficial effect of the present invention is: add different sequestrants, it act as and contributes to the slow releasing of metal ion in reaction process, thus make the process of generation lanthanum, yttrium and cerium element co-doped bismuth vanadium pigments compare the carrying out of mitigation, the bismuth vanadium pigments chemical constitution obtained is even, particle diameter is less, and within the scope of certain particle size, particle diameter is less, its opacifying power, tinting strength are stronger, from but the dominant hue of pigment and brightness improve; Microwave-hydrothermal method is used to prepare the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, its synthesis temperature is lower, generated time is shorter, and synthesis temperature needed for conventional solid-state method synthesis bismuth vanadium pigments is higher, generated time is longer, therefore, preparation method provided by the present invention is conducive to reducing energy consumption, reduces production cost; The product that the present invention finally obtains is the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, utilize lanthanum, yttrium and cerium element doped with the color generation property helping improve bismuth vanadium pigments, because the atomic structure of rare earth element uniqueness, the existence of the 4f electronic shell be not namely full of, when being subject to rayed, 4f electronic shell, to the characteristic with selective absorbing and reflection of light, due to this characteristic, can make rare earth doped beramic color have the advantage that color development is stablized, 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 0.1mmol(0.0325g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 160 DEG C, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.1mmol(0.0325g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 220 DEG C, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.1mmol(0.0325g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 160 DEG C, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.5mmol(0.1625g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 220 DEG C, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.5mmol(0.1625g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 160 DEG C, and microwave hydrothermal 1h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.5mmol(0.1625g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 220 DEG C, and microwave hydrothermal 3h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.3mmol(0.0975g wherein) La (NO 3) 3, 0.3mmol(0.1149g) Y (NO 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 185 DEG C, and microwave hydrothermal 2h.Then, with deionized water and absolute ethanol washing several times, dry 12h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, 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 0.4mmol(0.13216g wherein) 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 is carried out mixing and is forwarded in water heating kettle after abundant stirring, at 200 DEG C, and microwave hydrothermal 2.5h.Then, with deionized water and absolute ethanol washing several times, dry 1.5h at 60 DEG C in vacuum drying oven subsequently, obtain the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped, its general formula is Bi 0.76la 0.08y 0.08ce 0.08vO 4.
In the present invention, with the addition of different sequestrants, effectively can control speed of reaction, make the carrying out of the process gentleness of generation 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 effectively can shorten preparation time to carry out the preparation of bismuth vanadium pigments.

Claims (5)

1. lanthanum, yttrium and a 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;
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 3carry out fully stirring obtaining solution A, wherein Bi (NO in solution 3) 35H 2o, La (NO 3) 3, Y (NO 3) 36H 2o, Ce (NO 3) 36H 2o, HNO 3be 1:(0.02 ~ 0.1 with the mol ratio of sequestrant): (0.02 ~ 0.1): (0.02 ~ 0.1): (4 ~ 16): (0.5 ~ 2); By NaVO 32H 2o to be dissolved in the NaOH solution of 1 ~ 4mol/L and to carry out fully stirring obtaining solution B, wherein NaVO 32H 2the mol ratio of O and NaOH is 1:(4 ~ 16); Described sequestrant is ethylenediamine tetraacetic acid (EDTA), Trisodium Citrate, methyl ethyl diketone or several mixtures;
(2), solution A and solution B mixed and carry out fully stirring forming suspension, wherein Bi 3+and VO 3-mol ratio be 1:1, this suspension is the presoma of the bismuth vanadium pigments of lanthanum, yttrium and cerium element co-doped;
(3), by above-mentioned suspension be transferred in microwave hydrothermal instrument, utilize carry out microwave radiation heating; After microwave hydrothermal reacts completely, washing several times, the bismuth vanadium pigments of obtained lanthanum, yttrium and cerium element co-doped after vacuum-drying.
2. lanthanum according to claim 1, yttrium and cerium codoped pucherite mineral dye preparation method, it is characterized in that: suspension is transferred in microwave hydrothermal instrument in step (3), utilize carry out microwave radiation heating will to 160 DEG C ~ 220 DEG C, hydro-thermal reaction 1 ~ 3h.
3. lanthanum according to claim 1, 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.
4. lanthanum according to claim 1, yttrium and cerium codoped pucherite mineral dye preparation method, it is characterized in that: in step (3) after washing in vacuum drying oven dry 12h at 60 DEG C, the bismuth vanadium pigments of obtained lanthanum, yttrium and cerium element co-doped.
5., as lanthanum, yttrium and a cerium codoped pucherite mineral dye that claim 1-4 preparation method obtains, it is characterized in that: its general formula is Bi 1-x-y-zla xy yce zvO 4, wherein 0.02≤x≤0.1,0.02≤y≤0.1,0.02≤z≤0.1.
CN201310343674.7A 2013-08-08 2013-08-08 Lanthanum, yttrium and cerium co-doped bismuth vanadate inorganic pigment and preparation method thereof Active CN103449518B (en)

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CN109181369B (en) * 2018-10-15 2021-03-26 中国科学院兰州化学物理研究所 Microwave hydrothermal assisted method for preparing high-chroma cobalt blue/clay mineral hybrid pigment
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