CN110760202A - Preparation method of bismuth vanadate fluorescent pigment - Google Patents
Preparation method of bismuth vanadate fluorescent pigment Download PDFInfo
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- CN110760202A CN110760202A CN201910880873.9A CN201910880873A CN110760202A CN 110760202 A CN110760202 A CN 110760202A CN 201910880873 A CN201910880873 A CN 201910880873A CN 110760202 A CN110760202 A CN 110760202A
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a preparation method of bismuth vanadate fluorescent pigment, which comprises the following steps: s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I; s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II; s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor; s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction; s5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to prepare the bismuth vanadate fluorescent pigment material.
Description
Technical Field
The invention relates to the technical field of preparation of fluorescent pigments, in particular to a preparation method of bismuth vanadate fluorescent pigment.
Background
The fluorescent pigment has excellent performance in the aspects of coloring plastic cement, sol, paper products, color paste, printing ink, paint, coating, color master batch, chemical fiber, textile and the like, has visibility far superior to the traditional gloss under natural conditions and under the light conditions of dawn, dusk, fog climate, projection and the like, can attract attention earlier and faster, has longer time for holding the attention, greatly increases the chance of looking back at the second eye and even the third eye, and has more and more extensive commercial interests and obtains more and more extensive commercial application;
however, the existing bismuth vanadate fluorescent pigment has poor light resistance and solubility resistance, and poor vividness and coloring capability, so that the reflectivity of the pigment cannot be conveniently and rapidly recognized under the condition of light projection, and the visual effect is reduced.
Disclosure of Invention
The invention provides a preparation method of bismuth vanadate fluorescent pigment, which can effectively solve the problems that the existing bismuth vanadate fluorescent pigment has poor light resistance and solubility resistance, and poor vividness and coloring capability, so that the reflection degree of the pigment cannot be conveniently and rapidly identified under the condition of light projection, and the visual effect is reduced.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of bismuth vanadate fluorescent pigment comprises the following steps:
s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I;
s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II;
s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor;
s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction;
and S5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to obtain the bismuth vanadate fluorescent pigment material.
According to the technical scheme, the mole number of NaOH in the step S1 is 2-6 times of that of vanadium, and the fluorine and phosphorus compounds account for 10-20% of the mole amount of vanadium.
According to the technical scheme, the environment in the step S3 is PH 3-8, and the temperature is 50-95 ℃.
According to the technical scheme, in the step S4, the reaction temperature is controlled to be 50-200 ℃, the pressure is controlled to be 0.1-1MPa, and the reaction is carried out for 3-10 hours.
According to the technical scheme, in the step S5, washing is carried out for 2-3 times by using distilled water and ethanol, and drying is carried out for 4 hours at 105 ℃.
According to the above technical solution, the step S3 further includes the following steps:
a1, putting the solution II into a stirring tank, adding the solution I after the temperature of the solution II is reduced to room temperature, and adding the solution I while stirring;
a2, continuously stirring after the addition is finished, carrying out real-time observation on the solution during stirring, and sampling and visually observing the solution;
and A3, after stirring, pouring into a reaction kettle.
According to the above technical solution, the step S5 further includes the following steps:
b1, putting the bismuth vanadate fluorescent pigment material into a grinding machine, and screening the pigment after grinding;
b2, screening through a screening machine, wherein impurities and blocks are separately picked out in screening, the impurities are recycled, and the blocks are placed into a grinding machine for secondary grinding;
and B3, after the screening is finished, grinding the unqualified bismuth vanadate fluorescent pigment again, and putting the unqualified bismuth vanadate fluorescent pigment into a grinding machine for secondary grinding.
And B4, detecting after grinding, packaging after detection, intensively boxing after treatment, then placing in a storehouse, and labeling.
According to the technical scheme, the sieve used for the screening machine in the step B2 is 600 meshes;
in the step B4, the bismuth vanadate fluorescent pigment is colored by being coated on a pigment base plate, and the conventional bismuth vanadate fluorescent pigment is also colored, so that the vividness and the tinting strength can be directly and visually measured conveniently.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the step B1 is at room temperature and is in a solid state.
According to the technical scheme, the process of B4 needs to be carried out twice for the bismuth vanadate fluorescent pigment.
Compared with the prior art, the invention has the beneficial effects that: the invention has scientific and reasonable structure, compared with other synthesis methods, the synthesis method has the characteristics of high reaction rate, low energy consumption, high yield, suitability for low-cost mass production and the like, is suitable for popularization and use, ensures that the product has good fluorescent pigment performance by simply adding fluorine and phosphorus compounds, overcomes the defects of poor light resistance and solubility resistance of common inorganic fluorescent pigments, has the characteristics of bright color light, strong tinting strength, good light resistance, weather resistance and chemical stability, has important significance for popularization of application research of the materials in wider fields, and has bright prospect in the inorganic fluorescent yellow pigment industry.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic flow diagram of a preparation process of the present invention;
FIG. 2 is a flowchart illustrating step S3 according to the present invention;
FIG. 3 is a flowchart illustrating step S5 according to the present invention;
FIG. 4 is a comparative experimental chart of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1: as shown in fig. 1 to 3, the present invention provides a method for preparing bismuth vanadate fluorescent pigment, comprising the following steps:
s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I;
s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II;
s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor;
s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction;
and S5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to obtain the bismuth vanadate fluorescent pigment material.
According to the technical scheme, in the step S1, the mol number of NaOH is 5 times that of vanadium element, and the mol amount of fluorine and phosphorus compound is 10% of vanadium.
According to the above technical solution, the environment in step S3 is PH 7, and the temperature is 65 ℃.
According to the technical scheme, in the step S4, the reaction temperature is controlled at 100 ℃, the pressure is controlled at 0.7MPa, and the reaction is carried out for 4 hours.
According to the technical scheme, in the step S5, washing is carried out for 2 times by using distilled water and ethanol, and drying is carried out for 4 hours at 105 ℃.
According to the above technical solution, step S3 further includes the following steps:
a1, putting the solution II into a stirring tank, adding the solution I after the temperature of the solution II is reduced to room temperature, and adding the solution I while stirring;
a2, continuously stirring after the addition is finished, carrying out real-time observation on the solution during stirring, and sampling and visually observing the solution;
and A3, after stirring, pouring into a reaction kettle.
According to the above technical solution, step S5 further includes the following steps:
b1, putting the bismuth vanadate fluorescent pigment material into a grinding machine, and screening the pigment after grinding;
b2, screening through a screening machine, wherein impurities and blocks are separately picked out in screening, the impurities are recycled, and the blocks are placed into a grinding machine for secondary grinding;
and B3, after the screening is finished, grinding the unqualified bismuth vanadate fluorescent pigment again, and putting the unqualified bismuth vanadate fluorescent pigment into a grinding machine for secondary grinding.
And B4, detecting after grinding, packaging after detection, intensively boxing after treatment, then placing in a storehouse, and labeling.
According to the technical scheme, the sieve used by the screening machine in the step B2 is 600 meshes;
in the step B4, the bismuth vanadate fluorescent pigment is colored by being coated on a pigment base plate, and the conventional bismuth vanadate fluorescent pigment is also colored, so that the vividness and the tinting strength can be directly and visually measured conveniently.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the step B1 is at room temperature and is in a solid state.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the B4 needs to be processed twice.
Example 2: as shown in fig. 1 to 3, the present invention provides a method for preparing bismuth vanadate fluorescent pigment, comprising the following steps:
s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I;
s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II;
s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor;
s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction;
and S5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to obtain the bismuth vanadate fluorescent pigment material.
According to the technical scheme, in the step S1, the mol number of NaOH is 5 times that of vanadium element, and the mol amount of fluorine and phosphorus compound is 15% of vanadium.
According to the above technical solution, the environment in step S3 is PH 8, and the temperature is 95 ℃.
According to the technical scheme, in the step S4, the reaction temperature is controlled to be 70 ℃, the pressure is controlled to be 0.1MPa, and the reaction is carried out for 3 hours.
According to the technical scheme, in the step S5, washing is carried out for 3 times by using distilled water and ethanol, and drying is carried out for 4 hours at 105 ℃.
According to the above technical solution, step S3 further includes the following steps:
a1, putting the solution II into a stirring tank, adding the solution I after the temperature of the solution II is reduced to room temperature, and adding the solution I while stirring;
a2, continuously stirring after the addition is finished, carrying out real-time observation on the solution during stirring, and sampling and visually observing the solution;
and A3, after stirring, pouring into a reaction kettle.
According to the above technical solution, step S5 further includes the following steps:
b1, putting the bismuth vanadate fluorescent pigment material into a grinding machine, and screening the pigment after grinding;
b2, screening through a screening machine, wherein impurities and blocks are separately picked out in screening, the impurities are recycled, and the blocks are placed into a grinding machine for secondary grinding;
and B3, after the screening is finished, grinding the unqualified bismuth vanadate fluorescent pigment again, and putting the unqualified bismuth vanadate fluorescent pigment into a grinding machine for secondary grinding.
And B4, detecting after grinding, packaging after detection, intensively boxing after treatment, then placing in a storehouse, and labeling.
According to the technical scheme, the sieve used by the screening machine in the step B2 is 600 meshes;
in the step B4, the bismuth vanadate fluorescent pigment is colored by being coated on a pigment base plate, and the conventional bismuth vanadate fluorescent pigment is also colored, so that the vividness and the tinting strength can be directly and visually measured conveniently.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the step B1 is at room temperature and is in a solid state.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the B4 needs to be processed twice.
Example 3: as shown in fig. 1 to 3, the present invention provides a method for preparing bismuth vanadate fluorescent pigment, comprising the following steps:
s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I;
s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II;
s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor;
s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction;
and S5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to obtain the bismuth vanadate fluorescent pigment material.
According to the technical scheme, in the step S1, the mol number of NaOH is 2 times that of vanadium element, and the mol amount of fluorine and phosphorus compound is 20% of vanadium.
According to the above technical solution, the environment in step S3 is PH 3, and the temperature is 80 ℃.
According to the technical scheme, in the step S4, the reaction temperature is controlled to be 130 ℃, the pressure is controlled to be 0.1MPa, and the reaction is carried out for 10 hours.
According to the technical scheme, in the step S5, washing is carried out for 2 times by using distilled water and ethanol, and drying is carried out for 4 hours at 105 ℃.
According to the above technical solution, step S3 further includes the following steps:
a1, putting the solution II into a stirring tank, adding the solution I after the temperature of the solution II is reduced to room temperature, and adding the solution I while stirring;
a2, continuously stirring after the addition is finished, carrying out real-time observation on the solution during stirring, and sampling and visually observing the solution;
and A3, after stirring, pouring into a reaction kettle.
According to the above technical solution, step S5 further includes the following steps:
b1, putting the bismuth vanadate fluorescent pigment material into a grinding machine, and screening the pigment after grinding;
b2, screening through a screening machine, wherein impurities and blocks are separately picked out in screening, the impurities are recycled, and the blocks are placed into a grinding machine for secondary grinding;
and B3, after the screening is finished, grinding the unqualified bismuth vanadate fluorescent pigment again, and putting the unqualified bismuth vanadate fluorescent pigment into a grinding machine for secondary grinding.
And B4, detecting after grinding, packaging after detection, intensively boxing after treatment, then placing in a storehouse, and labeling.
According to the technical scheme, the sieve used by the screening machine in the step B2 is 600 meshes;
in the step B4, the bismuth vanadate fluorescent pigment is colored by being coated on a pigment base plate, and the conventional bismuth vanadate fluorescent pigment is also colored, so that the vividness and the tinting strength can be directly and visually measured conveniently.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the step B1 is at room temperature and is in a solid state.
According to the technical scheme, the bismuth vanadate fluorescent pigment in the B4 needs to be processed twice.
As shown in fig. 4, the written fluorescent pigments prepared in examples 1, 2 and 3 were labeled as sample nos. 1, 2 and 3, and the unlabeled conventional bismuth vanadate pigment, and it can be seen from the pigment drawing that the bismuth vanadate fluorescent pigment has better color vividness and tinctorial strength.
Compared with the prior art, the invention has the beneficial effects that: the invention has scientific and reasonable structure, compared with other synthesis methods, the synthesis method has the characteristics of high reaction rate, low energy consumption, high yield, suitability for low-cost mass production and the like, is suitable for popularization and use, ensures that the product has good fluorescent pigment performance by simply adding fluorine and phosphorus compounds, overcomes the defects of poor light resistance and solubility resistance of common inorganic fluorescent pigments, has the characteristics of bright color light, strong tinting strength, good light resistance, weather resistance and chemical stability, has important significance for popularization of application research of the materials in wider fields, and has bright prospect in the inorganic fluorescent yellow pigment industry.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of bismuth vanadate fluorescent pigment is characterized in that: the method comprises the following steps:
s1, weighing ammonium metavanadate solid, fluorine and phosphorus compounds at room temperature, adding distilled water, adding NaOH, and intensively stirring for 15 minutes to obtain a solution I;
s2, weighing bismuth nitrate solid according to the molar ratio of the bismuth nitrate solid to vanadium element, adding calcium nitrate, and adding a small amount of concentrated nitric acid for dissolution to obtain a bismuth nitrate solution II;
s3, adding the solution I into the solution II, and stirring for 1 hour to obtain a bismuth vanadate fluorescent pigment precursor;
s4, transferring the obtained mixed solution into a stainless steel reaction kettle for controlled reaction;
and S5, after the reaction is finished, washing the prepared product with distilled water and ethanol respectively, and then drying to obtain the bismuth vanadate fluorescent pigment material.
2. The method of claim 1, wherein the molar amount of NaOH is 2-6 times that of vanadium in step S1, and the fluorine and phosphorus compounds are 10-20 mol% of vanadium.
3. The method of claim 1, wherein the environment of step S3 is PH 3-8 and the temperature is 50-95 ℃.
4. The method of claim 1, wherein the reaction temperature is controlled to 50-200 ℃ and the pressure is controlled to 0.1-1MPa in step S4, and the reaction is carried out for 3-10 hours.
5. The method of claim 1, wherein the bismuth vanadate fluorescent pigment is washed with distilled water and ethanol for 2-3 times and dried at 105 ℃ for 4 hours in step S5.
6. The method for preparing bismuth vanadate fluorescent pigment according to claim 1, wherein the step S3 further comprises the following steps:
a1, putting the solution II into a stirring tank, adding the solution I after the temperature of the solution II is reduced to room temperature, and adding the solution I while stirring;
a2, continuously stirring after the addition is finished, carrying out real-time observation on the solution during stirring, and sampling and visually observing the solution;
and A3, after stirring, pouring into a reaction kettle.
7. The method for preparing bismuth vanadate fluorescent pigment according to claim 1, wherein the step S5 further comprises the steps of:
b1, putting the bismuth vanadate fluorescent pigment material into a grinding machine, and screening the pigment after grinding;
b2, screening through a screening machine, wherein impurities and blocks are separately picked out in screening, the impurities are recycled, and the blocks are placed into a grinding machine for secondary grinding;
and B3, after the screening is finished, grinding the unqualified bismuth vanadate fluorescent pigment again, and putting the unqualified bismuth vanadate fluorescent pigment into a grinding machine for secondary grinding.
And B4, detecting after grinding, packaging after detection, intensively boxing after treatment, then placing in a storehouse, and labeling.
8. The method for preparing bismuth vanadate fluorescent pigment according to claim 7, wherein the sieve used in the step B2 for the sieving machine is 600 mesh;
in the step B4, the bismuth vanadate fluorescent pigment is colored by being coated on a pigment base plate, and the conventional bismuth vanadate fluorescent pigment is also colored, so that the vividness and the tinting strength can be directly and visually measured conveniently.
9. The method of claim 7, wherein the bismuth vanadate fluorescent pigment in step B1 is in a solid state and at room temperature.
10. The method of claim 8, wherein the step of performing B4 for the bismuth vanadate fluorescent pigment is performed twice.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117384494A (en) * | 2023-10-13 | 2024-01-12 | 鞍钢集团北京研究院有限公司 | A method for optimizing the colorimetric properties of bismuth vanadate yellow inorganic pigment |
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