CN109370258B - Production method of vanadium-zirconium blue pigment with good color development effect - Google Patents
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- CN109370258B CN109370258B CN201811056200.3A CN201811056200A CN109370258B CN 109370258 B CN109370258 B CN 109370258B CN 201811056200 A CN201811056200 A CN 201811056200A CN 109370258 B CN109370258 B CN 109370258B
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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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
- C09C1/0012—Pigments for ceramics containing zirconium and silicon
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- 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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- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/66—Hue (H*)
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Abstract
The invention relates to the technical field of ceramic pigments, and aims to provide a production method of a vanadium-zirconium blue pigment, which comprises the following steps: step 1, mixing fluxing agent, binder and first toner and then granulating; step 2, carrying out smelting treatment on zircon sand and the product obtained in the step 1 at high temperature; step 3, grinding the fused zirconia obtained in the step 2; and 4, mixing and grinding other raw materials of the vanadium-zirconium blue and the product obtained in the step 3, heating, calcining, cooling and cooling to obtain the vanadium-zirconium blue pigment. The invention has the beneficial effects that: the zircon sand and the regulator are smelted at high temperature, the content of the toner in the fused zirconia and the granularity of the fused zirconia are controlled after smelting, and finally, other raw materials of the blue vanadium zirconium are added to produce the blue vanadium zirconium pigment, so that the produced blue vanadium zirconium pigment is blue, the requirements of daily ceramics and technical ceramics industries on blue and blue colors are met, and the color of the ceramic product is enriched.
Description
The scheme is divided into separate applications by taking an invention patent with the application date of 2017, 05 and 08, the application number of 201710315514.X and the name of 'a production method of a vanadium-zirconium blue pigment' as a parent application.
Technical Field
The invention relates to the technical field of ceramic pigments, in particular to a production method of a vanadium-zirconium blue pigment.
Background
The zirconium ceramic pigment has the excellent performances of bright color development and good miscibility, thereby playing an important role in the pigments for common glaze and blank of ceramics, wherein the most common and most used zirconium ceramic pigment is the three primary colors: the main crystal phase of the blue vanadium zirconium, zirconium praseodymium yellow and zirconium iron red is zirconium silicate, and the blue vanadium zirconium, the zirconium praseodymium yellow and the zirconium iron red are generated from zirconium oxide and quartz at high temperature. At present, the vanadium-zirconium blue pigment used in the daily ceramics and technical ceramics industries is biased to blue hue, while the vanadium-zirconium blue pigment prepared by common electric melting zirconia is dark blue hue, the color development effect of preparing the blue hue is not ideal, and the application requirement of the daily ceramics and technical ceramics industries on the blue hue vanadium-zirconium blue pigment can not be met. Therefore, it is necessary to provide a method for producing a blue material of vanadium zirconium which can give bluish hue.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for producing a vanadium-zirconium blue pigment which enables the color tone of the vanadium-zirconium blue to be blue.
In order to solve the technical problems, the invention adopts the technical scheme that:
a production method of a vanadium-zirconium blue pigment comprises the following steps:
step 1, mixing fluxing agent, adhesive and first toner according to the following parts by weight: 20-25 parts of fluxing agent, 5-10 parts of binder and 65-75 parts of first toner, and granulating after mixing to obtain second toner;
step 2, melting the zircon sand and the second toner obtained in the step 1 at the temperature of 2500-;
step 3, grinding the fused zirconia obtained in the step 2, and controlling the granularity of the fused zirconia to be 13-18 μm;
and 4, mixing and grinding the vanadium-zirconium colorant and the auxiliary material with the fused zirconia obtained in the step 3, uniformly heating for 8-10 hours to 750-850 ℃ after grinding, then preserving heat for 2 hours, cooling and taking out to obtain the vanadium-zirconium blue pigment.
Further, in the step 1, a granulator is used for granulation treatment, and the granulation particle size is controlled to be 1-2 mm.
Further, in the step 2, the obtained fused zirconia is subjected to spectrum measurement, and when the mass fraction of the toner in the fused zirconia is less than 0.3%, the operation of the step 2 is continued until the mass fraction of the toner in the fused zirconia is 0.3% -0.8%.
Further, the mass fraction of the toner in the fused zirconia obtained in the step 2 is 0.3% -0.5%.
Further, in the step 3, the particle size is controlled by grinding with a ball mill and observing and controlling with a laser particle size analyzer.
Further, in the step 4, the mass fraction of the fused zirconia in the obtained vanadium-zirconium blue pigment is 50-60%.
Further, the temperature of the heat preservation in the step 4 is 800 ℃.
The invention has the beneficial effects that: smelting zircon sand and a toner at high temperature to obtain fused zirconia, controlling the content of the toner in the fused zirconia, controlling the granularity of the fused zirconia to meet the requirement of color development of color tone, and finally adding a colorant of vanadium-zirconium blue and other auxiliary raw materials to prepare the vanadium-zirconium blue pigment; the produced blue pigment of vanadium zirconium is blue, changes the dark blue color tone of the blue pigment of vanadium zirconium prepared by the prior electric melting zirconia, meets the requirements of the industries of daily ceramics and technical ceramics on the blue color tone, and enriches the color of the ceramic product.
Drawings
FIG. 1 is a process flow diagram of a method for producing a blue pigment of vanadium zirconium in accordance with an embodiment of the present invention.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the present invention in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the embodiments.
The most key concept of the invention is as follows: the toner and zircon sand are smelted at high temperature to obtain the fused zirconia, the granularity of the fused zirconia and the content of a second toner in the fused zirconia are controlled, so that the fused zirconia has a good color development effect, and the produced blue material of the vanadium zirconium is blue.
Referring to fig. 1, the method for producing a blue material containing vanadium and zirconium of the present embodiment includes the following steps:
step 1, mixing fluxing agent, adhesive and first toner according to the following parts by weight: 20-25 parts of fluxing agent, 5-10 parts of binder and 65-75 parts of first toner, and granulating in a granulator after completely mixing to obtain second toner and finish the preparation of the toner;
step 2, smelting zircon sand and the second toner obtained in the step 1 at the temperature of 2500-;
step 3, grinding the fused zirconia obtained in the step 2, controlling the granularity of the fused zirconia to be 13-18 microns, detecting the granularity, performing subsequent operation if the granularity meets the requirement, and continuing grinding if the granularity does not meet the requirement;
and 4, mixing a vanadium-zirconium colorant (vanadium pentoxide) and auxiliary materials (industrial salt, quartz powder and the like) with the fused zirconia obtained in the step 3, grinding, uniformly heating for 8-10 hours to 750-fold at 850 ℃, then preserving heat for 2 hours, cooling and taking out to obtain a vanadium-zirconium blue pigment, thereby completing the preparation of the sample.
From the above description, the beneficial effects of the present invention are: after zircon sand and a toner are smelted at high temperature, fused zirconia is obtained, the content of the toner in the fused zirconia and the granularity of the fused zirconia are controlled so as to meet the requirement of color development of color tones, and finally, other raw materials of vanadium-zirconium blue, such as vanadium pentoxide, industrial salt and the like, are added to prepare the vanadium-zirconium blue pigment; the produced blue pigment of vanadium zirconium is blue, which changes the dark blue color tone of the blue pigment of vanadium zirconium prepared by the prior electric melting zirconia, meets the requirements of the industries of domestic ceramics and technical ceramics on the blue color tone and enriches the color of the ceramic product;
further, in the step 1, a granulator is used for granulation treatment, and the granulation particle size is controlled to be 1-2 mm.
As is apparent from the above description, the toner is controlled to have a particle size of 1 to 2mm, and the toner can be sufficiently fused with zircon sand.
Further, in the step 2, the obtained fused zirconia is subjected to spectrum measurement, and when the mass fraction of the toner in the fused zirconia is less than 0.3%, the operation of the step 2 is continued until the mass fraction of the toner in the fused zirconia is 0.3% -0.8%.
Further, the mass fraction of the toner in the fused zirconia obtained in the step 2 is 0.3% -0.5%.
As can be seen from the above description, the spectral measurement mainly detects the contents of zirconia, silica, alumina, and titania in the fused zirconia, so as to determine the chemical component contents of the fused zirconia, and then obtain the toner in the fused zirconia; the control of the content of the toner mainly adjusts the tone of blue, and when the mass fraction of the toner in the fused zirconia is 0.3-0.5%, a better color development effect is achieved.
Further, in the step 3, the particle size is controlled by grinding with a ball mill and observing and controlling with a laser particle size analyzer.
From the above description, the laser particle size analyzer can accurately control the grinding particle size of the fused zirconia.
Further, in the step 4, the mass fraction of the fused zirconia in the obtained vanadium-zirconium blue pigment is 50-60%.
From the above description, it can be known that the content of the fused zirconia in the blue material of the vanadium zirconium is 50% -60%, so that the ratio of the fused zirconia to other raw materials of the vanadium zirconium blue is optimal, and the prepared vanadium zirconium blue meets the requirement of color development.
Further, the temperature of the heat preservation in the step 4 is 800 ℃.
As can be seen from the above description, the reaction temperature of the blue material of vanadium zirconium at 800 ℃ is preferred, so that the reaction of the materials in the preparation process is complete.
Referring to fig. 1, a first embodiment of the present invention is:
a production method of a vanadium-zirconium blue pigment comprises the following steps:
step 1, mixing fluxing agent, adhesive and first toner according to the following parts by weight: 25 parts of fluxing agent (sodium fluoride), 5 parts of binding agent (sodium silicate) and 70 parts of toner (lithium carbonate), uniformly mixing by a stirrer, and then granulating in a granulator, wherein the grain size of the granules is controlled to be 1mm, so as to obtain second toner;
step 2, after the zircon sand and the second toner obtained in the step 1 are smelted at 2750 ℃, cooling with industrial water, drying at 150 ℃ for later use, performing spectral measurement on the fused zirconia after high-temperature smelting, and when the content of the toner in the fused zirconia is less than 0.3%, continuing to smelt the fused zirconia at high temperature until the content of the toner in the added fused zirconia is 0.4%, so as to obtain the fused zirconia;
step 3, grinding the fused zirconia obtained in the step 2 by using ball milling equipment, observing and controlling by using a laser particle size analyzer, and controlling the particle size of the fused zirconia to be 15 microns;
and 4, mixing a vanadium-zirconium colorant (vanadium pentoxide) and auxiliary materials (industrial salt, quartz powder and sodium fluoride) with the fused zirconia obtained in the step 3, grinding, wherein the auxiliary materials are used for synthesizing a vanadium-zirconium blue pigment at a lower temperature, uniformly heating the vanadium-zirconium blue pigment in a calcining furnace for 9 to 800 ℃ after grinding, then keeping the temperature at 800 ℃ for 2 hours, cooling and taking out the vanadium-zirconium blue pigment to obtain the vanadium-zirconium blue pigment, wherein the mass fraction of the fused zirconia in the vanadium-zirconium blue pigment is 60%.
The second embodiment of the invention is as follows:
a production method of a vanadium-zirconium blue pigment comprises the following steps:
step 1, mixing fluxing agent, adhesive and first toner according to the following parts by weight: 20 parts of fluxing agent (potassium chloride), 5 parts of binding agent (sodium silicate) and 75 parts of toner (sodium carbonate), uniformly mixing by a stirrer, and then granulating in a granulator, wherein the grain size of the granules is controlled to be 2mm, so as to obtain second toner;
step 2, melting zircon sand and the second toner obtained in the step 1 at 2500 ℃, cooling with industrial water, drying at 100 ℃ for later use, performing spectral measurement on the fused zirconia after high-temperature melting, and continuing to perform high-temperature melting on the fused zirconia when the content of the toner in the fused zirconia is less than 0.3% until the content of the toner in the added fused zirconia is 0.5%, so as to obtain the fused zirconia;
step 3, grinding the fused zirconia obtained in the step 2 by using ball milling equipment, observing and controlling by using a laser particle size analyzer, and controlling the particle size of the fused zirconia to be 13 mu m;
and 4, mixing a vanadium-zirconium colorant (vanadium pentoxide) and auxiliary materials (industrial salt, quartz powder and sodium fluoride) with the fused zirconia obtained in the step 3, grinding, wherein the auxiliary materials are used for synthesizing a vanadium-zirconium blue pigment at a lower temperature, uniformly heating the vanadium-zirconium blue pigment in a calcining furnace for 10 to 850 ℃ after grinding, then keeping the temperature at 800 ℃ for 2 hours, cooling and taking out the vanadium-zirconium blue pigment to obtain the vanadium-zirconium blue pigment, wherein the mass fraction of the fused zirconia in the vanadium-zirconium blue pigment is 50%.
The color development test shows that the effect of the invention is good, the prepared vanadium-zirconium blue pigment is ground into a 350-mesh powder product, the powder product is added into ceramic glaze according to the mass fraction of 5 percent, then the ceramic is sintered at 1250 ℃, and the color development effect is tested by a color difference meter after cooling.
The treated blue material of vanadium and zirconium is subjected to color development experiments, the experimental results are shown in table 1,
TABLE 1 comparison table of color difference values of color development of vanadium zirconium blue pigment
The color development experiment results in table 1 show that the color development tone of the vanadium zirconium blue pigment produced by the electrofused zirconia added with the toner is obviously changed, the color development quality is better than that of a standard sample, and the color development tone is suitable for the required effect of domestic ceramics and technical ceramics.
In conclusion, according to the production method of the vanadium-zirconium blue pigment, provided by the invention, the grain size of granulation is controlled during preparation of the regulator, so that the prepared toner and zircon sand can be fully fused during high-temperature smelting; controlling the content of the toner in the smelted zirconia and adjusting the content of the toner through spectral measurement; the particle size of the fused zirconia and the content of the toner in the fused zirconia are controlled, so that the produced blue vanadium zirconium is in a better color development effect, other raw materials of the blue vanadium zirconium are added, and the related reaction temperature is controlled to produce the blue vanadium zirconium pigment, so that the produced blue vanadium zirconium pigment is in a blue tone, and the dark blue tone of the blue vanadium zirconium pigment prepared by the original fused zirconia is changed; the color development tone of the vanadium zirconium blue pigment produced by the fused zirconia added with the toner is obviously changed, the color development quality is better than that of a standard sample, the requirement of the domestic ceramic and technical ceramic industry on the blue tone is met, and the color of the ceramic product is enriched.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The production method of the vanadium-zirconium blue pigment with good color development effect is characterized by comprising the following steps:
step 1, mixing fluxing agent, adhesive and first toner according to the following parts by weight: 25 parts of fluxing agent, 5 parts of binder and 70 parts of first toner, and granulating after mixing to obtain a second toner;
the fluxing agent is sodium fluoride, the binder is sodium silicate, and the first toner is lithium carbonate;
step 2, melting the zircon sand and the second toner obtained in the step 1 at the temperature of 2500-;
the mass fraction of the second toner in the electrofused zirconia is 0.4%;
step 3, grinding the fused zirconia obtained in the step 2, and controlling the granularity of the fused zirconia to be 15 microns;
and 4, mixing the vanadium-zirconium colorant and the auxiliary material with the fused zirconia obtained in the step 3, grinding, uniformly heating for 9 hours to 800 ℃ after grinding, then preserving heat for 2 hours, cooling and taking out to obtain the vanadium-zirconium blue pigment.
2. The method for producing a vanadium zirconium blue colorant having a good coloring effect according to claim 1, wherein: in the step 1, a granulator is used for granulation treatment, and the granulation particle size is controlled to be 1-2 mm.
3. The method for producing a vanadium zirconium blue colorant having a good coloring effect according to claim 1, wherein: in the step 3, the granularity is controlled by grinding through ball milling equipment, and is observed and controlled by a laser granularity meter.
4. The method for producing a vanadium zirconium blue colorant having a good coloring effect according to claim 1, wherein: in the step 4, the mass fraction of the fused zirconia in the obtained vanadium-zirconium blue pigment is 50-60%.
5. The method for producing a vanadium zirconium blue colorant having a good coloring effect according to claim 1, wherein: the heat preservation temperature in the step 4 is 800 ℃.
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| CN201811056200.3A CN109370258B (en) | 2017-05-08 | 2017-05-08 | Production method of vanadium-zirconium blue pigment with good color development effect |
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| CN201710315514.XA CN107118589B (en) | 2017-05-08 | 2017-05-08 | A kind of production method of zircon-vanadium blue pigment |
| CN201811056200.3A CN109370258B (en) | 2017-05-08 | 2017-05-08 | Production method of vanadium-zirconium blue pigment with good color development effect |
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| CN108250804B (en) * | 2018-01-31 | 2020-05-05 | 洛阳师范学院 | Nano vanadium-zirconium blue ceramic pigment and preparation method thereof |
| CN111849207B (en) * | 2020-08-13 | 2021-09-10 | 三祥新材股份有限公司 | Method for improving blue value of vanadium-zirconium blue pigment |
| CN113264673A (en) * | 2021-06-08 | 2021-08-17 | 三祥新材股份有限公司 | Method for producing yellowish-red zirconium-iron-red regulating pigment by electrically melting zirconia |
| CN113248254A (en) * | 2021-06-08 | 2021-08-13 | 三祥新材股份有限公司 | Method for improving temperature resistance of vanadium-zirconium blue pigment produced by electrically-fused zirconia |
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| JPH02254472A (en) * | 1989-03-28 | 1990-10-15 | Minolta Camera Co Ltd | Solid-state scanning type optical printing head |
| CN100387546C (en) * | 2003-05-09 | 2008-05-14 | 郑州大学 | Method for preparing alumine base electric fused zirconium corundum |
| DE10354346A1 (en) * | 2003-11-20 | 2005-07-14 | Schott Ag | Non-magnetic, ceramic one-component toner |
| CN102050640B (en) * | 2009-11-06 | 2013-10-23 | 佛山市华南精细陶瓷技术研究开发中心 | Method for preparing zircon-vanadium blue ceramic pigment |
| CN102173428B (en) * | 2011-03-04 | 2012-08-22 | 景德镇陶瓷学院 | Blue zirconium silicate pigment for spray ink printing and preparation method of blue zirconium silicate pigment |
| CN102225873B (en) * | 2011-04-11 | 2013-03-06 | 三祥新材股份有限公司 | Process for controlling crystal form of zirconia and improving chromogenic effect of pigment |
| CN103011906B (en) * | 2013-01-16 | 2015-02-11 | 焦作市科力达科技有限公司 | Production method of zirconium vanadium blue |
| CN104529541B (en) * | 2014-12-05 | 2016-05-04 | 三祥新材股份有限公司 | The preparation method of a kind of modification electric-melting zirconia and pr-yellow material |
| CN108624087B (en) * | 2016-01-26 | 2020-10-27 | 三祥新材股份有限公司 | Pretreatment method of zircon powder with high reaction activity |
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Non-Patent Citations (1)
| Title |
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| "Design of experiments with mixture variables as a tool for the formulation of pigments: The case of the blue (V-ZrSiO4)";Cabrelon, Marcelo D. 等;《CFI-CERAMIC FORUM INTERNATIONAL》;20061231;第83卷(第11-12期);E40-E46 * |
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| CN109233339A (en) | 2019-01-18 |
| CN107118589B (en) | 2018-11-13 |
| CN109233339B (en) | 2020-08-28 |
| CN107118589A (en) | 2017-09-01 |
| CN109370258A (en) | 2019-02-22 |
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