CN110683578A - Production method of high-activity electrofused zirconia - Google Patents
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Abstract
The invention relates to a pigment production technology, in particular to a production method of high-activity electrofusion zirconia applied in the field of high-end zirconium ceramic pigments. The method comprises the following steps: step 1), carrying out high-temperature desiliconization treatment on zircon sand to obtain fused zirconia hollow sphere particles; step 2) mixing the fused zirconia hollow sphere particles obtained in the step 1), the fused zirconia balls and water, and feeding the mixture into a stirring mill for grinding to obtain zirconia slurry; step 3) drying treatment: and 2) stirring the zirconia slurry obtained in the step 2) and an active agent solution, and granulating and drying by adopting a spray drying tower to obtain the high-activity fused zirconia. The invention has the beneficial effects that: the fused zirconia zirconium powder produced by the production method of the high-activity fused zirconia has high reaction activity, the tinting strength of the prepared ferrozirconium red pigment is obviously improved under the high-temperature condition, the ferrozirconium red pigment can replace chemical zirconium to produce the ferrozirconium red pigment, and the production cost of the ferrozirconium red pigment is reduced.
Description
Technical Field
The invention relates to a pigment production technology, in particular to a production method of high-activity electrofusion zirconia applied in the field of high-end zirconium ceramic pigments.
Background
Because the defect of poor reaction activity of common fused zirconia restricts the application of the fused zirconia in the field of high-end zirconium ceramic pigments, the high-end zirconium ceramic pigments are mostly made of chemical zirconium, such as ferrozirconium red pigments, inkjet praseodymium yellow pigments and the like. When the ceramic pigment made of the common electrofused zirconia is used at the temperature of over 1250 ℃, the fading is obvious, the coloring power is poor, namely, the temperature resistance can not reach the using effect of the pigment produced by chemical zirconium, and the using range of the electrofused zirconia is limited. The method has great relation with the poor activity of the common electrofused zirconia powder, the poor activity of the electrofused zirconia, the low activity, the narrow sintering range and the insufficient reaction in the reaction process of preparing the pigment, and the coloring elements can not be completely filled into the zirconium silicate lattice in the pigment synthesis process, so that the coloring power of the pigment is weakened, and the coloring effect is poor when the pigment is used in the field of high-end zirconium pigments.
Disclosure of Invention
The invention aims to provide a production method of high-activity electrofused zirconia, which improves the application performance of the electrofused zirconia in the field of high-end zirconium ceramic pigments.
In order to solve the technical problems, the invention adopts the technical scheme that: the production method of the high-activity electrofused zirconia comprises the following steps:
step 1), carrying out high-temperature desiliconization treatment on zircon sand to obtain fused zirconia hollow sphere particles; the high-temperature desiliconization temperature is about 2600 ℃ to 2750 ℃;
step 2) mixing the fused zirconia hollow sphere particles obtained in the step 1), the fused zirconia balls and water, and feeding the mixture into a stirring mill for grinding to obtain zirconia slurry;
the mass ratio of the fused zirconia hollow sphere particles to the fused zirconia balls to the water is 1-1.1: 3-3.3: 0.6-0.7; the particle size distribution of the zirconia slurry is as follows: d50 is controlled to be 1-1.5 μm, D90 is controlled to be 2.5-3 μm;
step 3) drying treatment: stirring the zirconia slurry obtained in the step 2) and an activator solution for 2-3 hours according to the mass ratio of 100:0.5-0.8, and then granulating and drying by adopting a spray drying tower to obtain the high-activity fused zirconia.
The invention has the beneficial effects that: the production method of the high-activity electrofused zirconia of the invention is characterized in that the zircon sand is desiliconized, i.e. the zirconia is separated from the silicon dioxide under the high-temperature condition; and grinding the cooled zirconia hollow spheres to obtain zirconia powder suitable for preparing a ferrozirconium red material, and dispersing and granulating the zirconia powder to improve the physical properties such as specific surface area, flowability and the like of the fused zirconia. The electrofused zirconia zirconium powder produced by the treatment means has high reaction activity, the tinting strength of the prepared ferrozirconium red material is obviously improved under the high-temperature condition, the ferrozirconium red material can replace chemical zirconium to produce the ferrozirconium red material, and the production cost of the ferrozirconium red material is reduced.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The invention provides a production method of high-activity electrofused zirconia, which comprises the following steps:
step 1), carrying out high-temperature desiliconization treatment on zircon sand to obtain fused zirconia hollow sphere particles; the high-temperature desiliconization temperature is about 2600 ℃ to 2750 ℃;
step 2) mixing the fused zirconia hollow sphere particles obtained in the step 1), the fused zirconia balls and water, and feeding the mixture into a stirring mill for grinding to obtain zirconia slurry;
the mass ratio of the fused zirconia hollow sphere particles to the fused zirconia balls to the water is 1-1.1: 3-3.3: 0.6-0.7; the particle size distribution of the zirconia slurry is as follows: d50 is controlled to be 1-1.5 μm, D90 is controlled to be 2.5-3 μm;
step 3) drying treatment: stirring the zirconia slurry obtained in the step 2) and an activator solution for 2-3 hours according to the mass ratio of 100:0.5-0.8, and then granulating and drying by adopting a spray drying tower to obtain the high-activity fused zirconia.
Further, in the method for producing high-activity electrofused zirconia, the solute of the active agent solution in the step 3) is prepared from organic matters and inorganic compounds according to the ratio of 3: 7, the organic matter is one or two of polyacrylamide or organic silicon oil, and the organic matter is one or more of sulfate, dilute sulfuric acid or zirconium oxychloride.
From the above description, it is known that the organic substance acts as a dispersing function and the inorganic compound acts as a surface modification function, further improving the specific surface area and the fluidity of the fused zirconia.
Further, in the method for producing high-activity electrofused zirconia, the method for preparing the activator solution in the step 3) comprises the following steps: and pouring the solute of the active agent solution into a stirring barrel, wherein the mass ratio of the solute of the active agent solution is as follows: stirring for 0.5-1 hr at a ratio of 1: 50.
Further, in the production method of the high-activity electrofused zirconia, the particle size of the electrofused zirconia slurry is observed and controlled by a malvern laser particle size analyzer in the step 2).
Further, in the method for producing the high-activity electrofused zirconia, the drying temperature of the spray drying tower in the step 3) is 200-250 ℃.
Example 1
The embodiment provides a production method of high-activity electrofused zirconia, which comprises the following steps:
step 1) zircon sand high-temperature desiliconization treatment: carrying out melting desiliconization treatment on the zircon sand material in a high-temperature electric arc furnace at 2600 ℃, and rapidly cooling to prepare electric melting zirconia hollow particles;
step 2) grinding treatment: feeding the hollow particles obtained in the step 1) into a stirring mill through a feeder to grind, and controlling the mass ratio of the hollow particles to zirconium balls to water, wherein the mass ratio is as follows: zirconium ball: water 1: 3:0.6, strictly controlling the particle size distribution of the zirconia slurry, mainly controlling D50 and D90, and controlling the particle size D50 of the slurry to be about 1.2 mu m and the particle size D90 to be about 2.6 mu m.
The zirconium balls are ceramic grinding balls which are prepared by firing chemical zirconium as a main material at a temperature of 1650 ℃, have the characteristics of high strength, high wear resistance and the like, and are often used as grinding media for grinding materials with high hardness, such as fused zirconia and the like.
Step 3) preparation of an active agent solution: adding a solute used as an active agent solution into water at normal temperature according to the proportion of 1:50, and uniformly stirring to prepare a solution for later use;
the solute of the active agent solution is prepared from organic compounds and inorganic compounds according to the weight ratio of 3: 7, the organic matter is polyacrylamide and organic silicon oil with the same quantity, and the organic matter is sulfate.
Step 4) zirconium powder activation treatment: uniformly adding the activator solution in the step 3) into the zirconia slurry in the step 2) according to the proportion of 0.6:100, and fully stirring for 1 hour for later use.
Step 5), preparing a zirconia powder sample: and (4) drying the fused zirconia mixed slurry obtained in the step 4) by adopting a spray drying tower, and controlling the temperature of the spray drying tower to be 200 ℃ to obtain the fused zirconia powder.
Effect testing
1. The specific surface areas of the respective samples are shown in table 1, and the fused zirconia powder obtained by the treatment in example 1 has a significantly larger specific surface area than that before the treatment, and is close to the specific surface area of chemical zirconium.
Ground fused zirconia: example 1 the ground electrofused zirconia dried powder obtained in step 2;
the treated fused zirconia is as follows: example 1, fused zirconia powder obtained in step 5);
the chemical zirconium 1 is: zibo general chemical zirconium;
the chemical zirconium 2 is: jiangxi Jingan chemical zirconium.
TABLE 1
| Serial number | Sample name | BET specific surface area (M)2/G) |
| 1 | Ground fused zirconia | 1.85 |
| 2 | Treated fused zirconia powder | 2.28 |
| 3 | Chemical zirconium 1 | 2.39 |
| 4 | Chemical zirconium 2 | 2.45 |
2. The application performance test of the high-activity zirconia obtained by the invention comprises the following steps: weighing each sample 1-4 in the sequence number table 1 and other auxiliary raw materials of the ferrozirconium red material (the auxiliary materials are mainly silicon dioxide, iron oxide red, magnesium fluoride, potassium chloride and the like, wherein zirconium oxide accounts for about 55%, silicon dioxide accounts for about 28%, iron oxide red accounts for about 10%, magnesium fluoride accounts for about 3.5%, and potassium chloride accounts for 3.5%), fully and uniformly mixing, grinding by a dry method for 20 minutes, canning, sealing and calcining at a constant speed for 6 hours at 1080 ℃, preserving heat for 2 hours when the temperature reaches 1000-. And then carrying out color development comparison on the zirconium iron red pigment.
The prepared ferrozirconium red material is subjected to color development experiments, and the results are shown in table 2, wherein the color development experiment results show that the effect is obviously improved compared with the effect before treatment, and the color development chromatic aberration of the ferrozirconium red material is close to that of the ferrozirconium red material prepared by chemical zirconium.
TABLE 2
In conclusion, the production method of the high-activity fused zirconia effectively increases the specific surface area of the fused zirconia powder through the later-stage dispersion modification treatment of the fused zirconia, and improves the dispersibility and the reaction activity of the fused zirconia, thereby improving the temperature resistance of the fused zirconia as the ferrozirconium red, completely replacing chemical zirconium to produce the ferrozirconium red material, and reducing the production cost of the high-end resistant zirconium ceramic pigment.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (5)
1. A production method of high-activity electrofused zirconia is characterized by comprising the following steps:
step 1), carrying out high-temperature desiliconization treatment on zircon sand to obtain fused zirconia hollow sphere particles; the high-temperature desiliconization temperature is about 2600 ℃ to 2750 ℃;
step 2) mixing the fused zirconia hollow sphere particles obtained in the step 1), the fused zirconia balls and water, and feeding the mixture into a stirring mill for grinding to obtain zirconia slurry;
the mass ratio of the fused zirconia hollow sphere particles to the fused zirconia balls to the water is 1-1.1: 3-3.3: 0.6-0.7; the particle size distribution of the zirconia slurry is as follows: d50 is controlled to be 1-1.5 μm, D90 is controlled to be 2.5-3 μm;
step 3) drying treatment: stirring the zirconia slurry obtained in the step 2) and an activator solution for 2-3 hours according to the mass ratio of 100:0.5-0.8, and then granulating and drying by adopting a spray drying tower to obtain the high-activity fused zirconia.
2. The method for producing a high-activity electrofused zirconia according to claim 1, wherein the solute of the active agent solution in the step 3) is composed of organic and inorganic compounds in a ratio of 3: 7, the organic matter is one or two of polyacrylamide or organic silicon oil, and the organic matter is one or more of sulfate, dilute sulfuric acid or zirconium oxychloride.
3. The method for producing high-activity electrofused zirconia according to claim 2, wherein the method for preparing the activator solution of step 3) comprises: and pouring the solute of the active agent solution into a stirring barrel, wherein the mass ratio of the solute of the active agent solution is as follows: stirring for 0.5-1 hr at a ratio of 1: 50.
4. The method for producing high-activity electrofused zirconia according to claim 1, wherein the particle size of the electrofused zirconia slurry is observed and controlled by a malvern laser particle sizer in the step 2).
5. The method for producing high-activity electrofused zirconia according to claim 1, wherein the drying temperature of the spray drying tower of the step 3) is 200-250 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393873A (en) * | 2020-03-24 | 2020-07-10 | 三祥新材股份有限公司 | Method for producing high-temperature-resistant zirconium ceramic pigment |
| CN111393874A (en) * | 2020-03-24 | 2020-07-10 | 三祥新材股份有限公司 | Method for producing high-temperature-resistant zirconium iron red pigment by electrically melting zirconia |
| CN111661874A (en) * | 2020-07-22 | 2020-09-15 | 三祥新材股份有限公司 | Method for reducing content of silicon oxide in fused zirconia powder |
| 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 |
Citations (1)
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| CN108384278A (en) * | 2018-03-06 | 2018-08-10 | 三祥新材股份有限公司 | A kind of production method of ink-jet pr-yellow material electric-melting zirconia |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108384278A (en) * | 2018-03-06 | 2018-08-10 | 三祥新材股份有限公司 | A kind of production method of ink-jet pr-yellow material electric-melting zirconia |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393873A (en) * | 2020-03-24 | 2020-07-10 | 三祥新材股份有限公司 | Method for producing high-temperature-resistant zirconium ceramic pigment |
| CN111393874A (en) * | 2020-03-24 | 2020-07-10 | 三祥新材股份有限公司 | Method for producing high-temperature-resistant zirconium iron red pigment by electrically melting zirconia |
| CN111661874A (en) * | 2020-07-22 | 2020-09-15 | 三祥新材股份有限公司 | Method for reducing content of silicon oxide in fused zirconia powder |
| 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 |
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Application publication date: 20200114 |