CN102775192B - Seed crystal introduced agate red ceramic pigment and preparation method thereof - Google Patents
Seed crystal introduced agate red ceramic pigment and preparation method thereof Download PDFInfo
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- CN102775192B CN102775192B CN201210236151.8A CN201210236151A CN102775192B CN 102775192 B CN102775192 B CN 102775192B CN 201210236151 A CN201210236151 A CN 201210236151A CN 102775192 B CN102775192 B CN 102775192B
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Abstract
The invention discloses a seed crystal introduced agate red ceramic pigment and a preparation method of the seed crystal introduced agate red ceramic pigment. The preparation method comprises the following steps of: (1) preparing seed crystals: evenly mixing calcium carbonate, stannic oxide, quartz and chrome green according to a molar ratio of (0.9-1.1):(0.9-1.1):(0.9-1.1):(0.115-0.135), mixing and grinding the obtained mixture, agate ball stone and water according to proportion by weight of 100:(450-550):(54-66) until the grain size achieves D90<=5mu m, drying and sieving the ground mixture, then adding boron-contained compounds which are 3%-5% of total weight, evenly mixing, burning, grinding and drying to obtain the seed crystals; and (2) preparing the pigment: evenly mixing calcium carbonate, stannic oxide, quartz and chrome green according to a molar ratio of (0.9-1.1):(0.9-1.1):(0.9-1.1):(0.115-0.135), adding the seed crystals which are 1%-3% of the total weight and the boron-contained compounds which are 3%-5% of the total weight, evenly mixing, burning, grinding and drying to obtain end products. The seed crystal introduced agate red ceramic pigment and the preparation method can reduce synthetic difficulties of the pigment and are strong in color development, bright in color and luster and good in thermostability.
Description
Technical field
The present invention relates to the production technical field of ceramic pigment, relate in particular to a kind of agate red ceramic pigment of introducing crystal seed and preparation method thereof.
Background technology
Chrome tin pink claims again agate red, is a kind of high temperature pigment of ceramic, because this colorant has stable crystalline structure, thereby can present beautiful agate red in the parent glaze adapting to.Chrome tin pink can be obtained to good decorative effect for wall brick, floor tile, sanitary china, because of but one of widely used colorant in current top-grade building, sanitary china goods.
But for a long time, it is quite weak that the research of the synthesis mechanism of people to agate red ceramic pigment seems, affects its synthetic factor very complicated again in addition, as long as middle slightly mistake of certain link all will affect the quality of final colorant.Therefore, the synthesis mechanism of research agate red ceramic pigment and the factor of the main colour generation of impact, determine best production process system, and tool is of great significance.
In the production process of agate red ceramic pigment, complexity and inlet that the synthetic difficulty of agate red ceramic pigment is mainly reflected in chromium and enters its aspidelite type lattice, the quantity that chromium enters tin tip stone is more, and colour generation is better, it is easier that chromium enters tin tip stone lattice, and synthesis technique is just got over easy handling.
Summary of the invention
In view of this, the object of the invention is to, a kind of preparation method of the agate red ceramic pigment of introducing crystal seed is provided, by introducing crystal seed, increase the resultant velocity of colorant, promote tin tip stone to generate, promote that chromium enters tin tip stone lattice.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method who introduces the agate red ceramic pigment of crystal seed, comprises the steps:
1) crystal seed preparation:
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, and obtains mixture; By mixture with agate ballstone, water by 100: (450～550): the weight ratio of (54～66) is mixed, ground, until particle diameter reaches D
90≤ 5um, then the mixture after grinding is dried, is sieved, then add the boron-containing compound that accounts for gross weight 3%～5% to mix, then calcine, grind, be dried, obtain crystal seed;
2) colorant preparation:
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, add again account for gross weight 1%-3%, step 1) crystal seed making and the boron-containing compound that accounts for gross weight 3%～5%, mix rear calcining, grinding, dry, get product.
Preferably, step 1) and step 2) in, the mol ratio of calcium carbonate, tindioxide, quartz, chrome green is 1: 1: 1: 0.125.
Preferably, step 1) and step 2) in be ground to and adopt the ball milling that carries out of ball mill.
Preferably, step 1) in the processing condition of calcining be: 30 ℃～500 ℃, intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～(1200-1300 ℃), intensification 5H; Constant temperature 5H at 1200 ℃～1300 ℃, then cooling naturally.
Preferably, step 2) in the processing condition of calcining be: 30 ℃～500 ℃, intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～1200 ℃, intensification 3H; Constant temperature 4H at 1200 ℃, is then cooled to below 200 ℃ naturally.
Preferably, step 1), step 2) in dry all at 150 ℃, carry out below.
Preferably, step 1) and step 2) in, the water ratio of dry rear mixture is less than 0.5%.
Preferably, step 1) in, after calcining, grind calcined material to particle diameter D
90reach 3～5mm.
Preferably, step 2) in, after calcining, grind calcined material to particle diameter D
90for 16mm～20mm.
Agate red ceramic pigment of the present invention, is made by aforementioned preparation method.
Compared with prior art, the present invention is owing to introducing crystal seed in the preparation process of agate red ceramic pigment, and fineness activity and the mixture homogeneity of the mode feed change by ball milling refinement while preparing crystal seed, because when pressed powder mixes, being less than the material that accounts for total amount 1% is to be difficult to evenly spread in system go, by the mode of ball milling refinement, the materials such as chromic oxide are uniformly distributed and fineness reaches refinement, according to the uniform material of solid state reaction mechanism altitude distribution, through calcining, more easily there is high temperature solid state reaction, so more easily form aspidelite type carrier, simultaneous oxidation chromium enters in lattice and goes more, product after calcining is through refinement, make particle diameter D
90reach 3～5mm, as crystal seed, the activity of crystal seed preparing is like this higher, for the preparation of agate red colorant, because preparation agate red colorant is when the high-temperature calcination, must be through multiple crystal conversion, the rise inducing action of the superfine crystal seed of this particle diameter to crystalline transformation, after adding, serve as the nucleus of crystal, nucleus is slowly grown up again, generate the crystal formation consistent with crystal seed, thereby make material generate more aspidelite type crystal structure carrier, chromium ion can enter in lattice more simultaneously, color development is strengthened, because aspidelite type carrier is completely synthetic, so high thermal resistance is good, red scale value is high, finally make stability improve.
Embodiment
Of the present invention being contemplated that: by introducing crystal seed in preparation process, reduce the synthetic difficulty of colorant, increase the stability of product quality simultaneously, make it in ceramic colour glaze color development stronger, color and luster is bright, and resistance to elevated temperatures is good.
In order to make those skilled in the art understand better technical scheme of the present invention, below in conjunction with by specific embodiment, the present invention is described in further detail.
The agate red ceramic pigment preparation method of introducing crystal seed of the present invention comprises two large steps, i.e. the preparation of synthetic, the colorant of crystal seed is specific as follows:
1, crystal seed preparation
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, and obtains mixture; By mixture with agate ballstone, water by 100: (450～550): the weight ratio of (54～66) is mixed, ground, until particle diameter reaches D
90≤ 5um, then the mixture after grinding is dried, is sieved, then add the boric acid that accounts for gross weight 3%～5%, mix then and calcine, grind, be dried, obtain crystal seed;
2, colorant preparation
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, add again account for gross weight 1%-3%, step 1) in the crystal seed that makes and the boric acid that accounts for gross weight 3%～5%, mix rear calcining, grinding, dry, get product.
The agate red ceramic pigment being made by above preparation method, has following characteristic:
Outward appearance: red-purple powder;
Lightness: 46≤L≤54;
Form and aspect: 24≤a≤29;
Form and aspect :-3≤b≤13.
Embodiments of the invention are as follows:
Embodiment mono-
1, crystal seed preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 preparation mixes;
2) press said mixture: agate ballstone: water=100: 500: 60; Ball mill ball milling approximately 72 hours, after ball milling, particle diameter reaches D
90≤ 5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio < 0.5%; To be dried thing and cross 325 eye mesh screens;
4) boric acid that is 99% by the mixture after above-mentioned sieving with concentration mixes and stirs by the mass ratio of 96.5: 3.5;
5) pack said mixture into potcal pot calcination, the processing condition of calcining are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1250, intensification 5H; Constant temperature 5H at 1250 ℃, naturally cooling;
6) by above-mentioned calcined material ball milling, particle diameter D
90reach 3-5um, dry (≤150 ℃), cross 325 eye mesh screens, are crystal seed finished product, standby;
2, colorant preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 mixes;
2) add the boric acid that crystal seed that step 1 makes and concentration are 99% to mix, the add-on of crystal seed accounts for crystal seed and boric acid adds 3% of rear mixture total weight amount again, and the add-on of boric acid accounts for crystal seed and boric acid adds 3.5% of rear mixture total weight amount;
3) said mixture is packed into 30 ℃～500 ℃ of potcal pot calcinations, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; Constant temperature 4H at 1200 ℃, naturally lowers the temperature 200 ℃ and unloads below.
4) by above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) cross 250 eye mesh screens, obtain agate red ceramic pigment.
The agate red ceramic pigment obtaining is above carried out to fineness and color development detection, and detected result is as follows:
1, fineness test
Test the data obtained: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development comparison and detection
The glaze colours basis glaze formula that agate red ceramic pigment is used:
0.276K
2O 0.003Fe
2O
3 3.5SiO
2
0.066Na
2O 0.522Al
2O
3 0.658CaO
In the present invention, in the synthetic colorant of the present invention who is 5% to additional massfraction in parent glaze and prior art, do not add the colorant product of crystal seed to do color development contrast, be labeled as respectively A and B, temperature of glaze firing is 1100 ℃, firing time is 60 minutes, soaking time 15-30 minute, and test color difference:
Test the data obtained: A sample: L:48.51 a:26.87 b:10.64.
Test the data obtained: B sample: L:50.34 a:21.56 b:8.99
Above data declaration the present embodiment is dark by the agate red ceramic pigment color development that adds crystal seed and prepare, and red scale value is high, and quality improves approximately 20%.
Embodiment bis-
1, crystal seed preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 preparation mixes;
2) press said mixture: agate ballstone: water=100: 500: 60; Ball mill ball milling approximately 78 hours, after ball milling, particle diameter reaches D
90≤ 5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio < 0.5%; To be dried thing and cross 325 eye mesh screens;
4) boric acid that is 99% by the mixture after above-mentioned sieving with concentration mixes and stirs by the mass ratio of 95: 5;
5) pack said mixture into potcal pot calcination, the processing condition of calcining are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1300 ℃, intensification 5H; Constant temperature 5H at 1300 ℃, naturally cooling;
6) by above-mentioned calcined material ball milling, particle diameter D
90reach 3-5um, dry (≤150 ℃), cross 325 eye mesh screens, are crystal seed finished product, standby;
2, colorant preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 1.1: 1.1: 1 in molar ratio: 0.115 mixes;
2) add the boric acid that crystal seed that step 1 makes and concentration are 99% again, mix, the add-on of crystal seed accounts for crystal seed and boric acid adds 5% of rear mixture total weight amount, and the add-on of boric acid accounts for crystal seed and boric acid adds 4% of rear mixture total weight amount;
3) said mixture is packed into 30 ℃～500 ℃ of potcal pot calcinations, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; 1200 ℃ of constant temperature 4H, naturally lower the temperature 200 ℃ and unload below.
4) by above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) cross 250 eye mesh screens, obtain agate red ceramic pigment.
The agate red ceramic pigment obtaining is above carried out to fineness and color development detection, and detected result is as follows:
1, fineness test
Test the data obtained: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development comparison and detection
The glaze colours basis glaze formula that agate red ceramic pigment is used:
0.216K
2O 0.003Fe
2O
3 3.5SiO
2
0.036Na
2O 0.622Al
2O
3 0.658CaO
In the present invention, the synthetic colorant of the present invention who is 5% to additional massfraction in parent glaze and do not add the product of crystal seed to do color development contrast, is labeled as respectively C and D, temperature of glaze firing is 1200 ℃, firing time is 60 minutes, soaking time 15-30 minute, and test color difference:
Test the data obtained: C sample: L:49.61 a:27.87 b:11.62.
Test the data obtained: D sample: L:53.51 a:15.26 b:18.12.
Above data declaration the present embodiment can be stablized color development by the agate red ceramic pigment that adds crystal seed and prepare in applied at elevated temperature situation, synthetic aspidelite N-type waferN more completely, resistance to elevated temperatures is good, and does not add D sample color development prepared by crystal seed to fade, color development poor stability.
Embodiment tri-
1, crystal seed preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 0.9: 1.1: 1 in molar ratio: 0.135 preparation mixes;
2) press said mixture and mix by the mass ratio of 100: 450: 56 with agate ballstone and water, use ball mill ball milling approximately 80 hours, after ball milling, particle diameter reaches D
90≤ 5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio < 0.5%; To be dried thing and cross 325 eye mesh screens;
4) boric acid that is 99% by the mixture after above-mentioned sieving with concentration mixes and stirs by the mass ratio of 95: 5;
5) pack said mixture into potcal pot calcination, the processing condition of calcining are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1300 ℃, intensification 5H; 1300 ℃ of constant temperature 5H, naturally cooling;
6) by above-mentioned calcined material ball milling, particle diameter D
90reach 3-5um, dry (≤150 ℃), cross 325 eye mesh screens, are crystal seed finished product, standby;
2, colorant preparation:
1) by calcium carbonate, tindioxide, quartz, chrome green 0.9: 1.1: 1 in molar ratio: 0.135 mixes;
2) add the boric acid that crystal seed that step 1 makes and concentration are 99% again, mix, the add-on of crystal seed accounts for crystal seed and boric acid adds 4% of rear mixture total weight amount, and the add-on of boric acid accounts for crystal seed and boric acid adds 3.5% of rear mixture total weight amount;
3) said mixture is packed into 30 ℃～500 ℃ of potcal pot calcinations, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; 1200 ℃ of constant temperature 4H, naturally lower the temperature 200 ℃ and unload below.
4) by above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) cross 250 eye mesh screens, obtain agate red ceramic pigment.
The agate red ceramic pigment obtaining is above carried out to fineness and color development detection, and detected result is as follows:
1, fineness test
Test the data obtained: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development detects
The glaze colours basis glaze formula that agate red ceramic pigment is used:
0.206K
2O 0.003Fe
2O
3 3.2SiO
2 0.712ZnO
0.036Na
2O 0.42Al
2O
3 0.621CaO
In the present invention, the synthetic colorant of the present invention who is 5% to additional massfraction in parent glaze and do not add the product of crystal seed to do color development contrast, is labeled as respectively E and F, temperature of glaze firing is 1100 ℃, firing time is 60 minutes, soaking time 15-30 minute, and test color difference:
Test the data obtained: E sample: L:50.31 a:27.87 b:10.64.
Test the data obtained: F sample: L:48.31 a:16.82 b:9.54.
Unsettled aspidelite type colorant there will be chromium stripping to react with the zinc oxide in glaze while using in containing the high glaze of zinc to cause colorant color development partially secretly partially green, red scale value reduction.Above data can find out that the agate red ceramic pigment that the present embodiment obtains can stablize color development in the glaze high containing zinc, red scale value is high, synthetic aspidelite type carrier colorant completely and can stable existence, and do not add the of the prior art common agate red colorant F sample color development of crystal seed dark, red scale value is low, unstable, the chromium ion in lattice has occurred to react with zinc oxide and has caused color development unstable.
By color development data, can be found out, the agate red colorant that the preparation method of the present embodiment makes can be stablized color development under high-temperature condition, color development is limpid simultaneously, red scale value is high, synthetic aspidelite type carrier energy stable existence when using containing the high glaze of zinc, there will not be chromium ion stripping and causes color development unstable.
Above the present invention is described in detail, applies specific case principle of the present invention and embodiment are set forth in literary composition, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (8)
1. a preparation method who introduces the agate red ceramic pigment of crystal seed, is characterized in that, comprises the steps:
1) crystal seed preparation:
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, and obtains mixture; By mixture with agate ballstone, water by 100:(450～550): the weight ratio of (54～66) is mixed, is ground, until particle diameter reaches D
90≤ 5 μ m, then the mixture after grinding is dried, is sieved, then add the boron-containing compound that accounts for gross weight 3%～5% to mix, then calcine, grind, be dried, obtain crystal seed;
2) colorant preparation:
By calcium carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes; add again the boron-containing compound that accounts for crystal seed gross weight 1%-3%, that step 1) makes and account for gross weight 3%～5%; mix rear calcining, grinding, dry, get product;
The processing condition of calcining in step 1) are: 30 ℃～500 ℃, and intensification 4h; 500 ℃～1000 ℃, intensification 4h; 1000 ℃～(1200-1300 ℃), intensification 5h; Constant temperature 5h at 1200 ℃～1300 ℃, then cooling naturally;
Step 2) in calcining processing condition be: 30 ℃～500 ℃, intensification 4h; 500 ℃～1000 ℃, intensification 4h; 1000 ℃～1200 ℃, intensification 3h; Constant temperature 4h at 1200 ℃, is then cooled to below 200 ℃ naturally.
2. preparation method as claimed in claim 1, is characterized in that, step 1) and step 2) in, the mol ratio of calcium carbonate, tindioxide, quartz, chrome green is 1:1:1:0.125.
3. preparation method as claimed in claim 1, is characterized in that, step 1) and step 2) in be ground to and adopt the ball milling that carries out of ball mill.
4. preparation method as claimed in claim 1, is characterized in that, step 1), step 2) in dry all at 150 ℃, carry out below.
5. preparation method as claimed in claim 1, is characterized in that, step 1) and step 2) in, the water ratio of dry rear mixture is less than 0.5%.
6. preparation method as claimed in claim 1, is characterized in that, in step 1), grinds calcined material to particle diameter D after calcining
90reach 3～5mm.
7. preparation method as claimed in claim 1, is characterized in that step 2) in, calcined material after calcining, ground to particle diameter D
90for 16mm～20mm.
8. an agate red ceramic pigment, is characterized in that, by the preparation method in claim 1～7, is made.
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| CN102992807A (en) * | 2012-11-26 | 2013-03-27 | 孙志勤 | Method for preparing agate red ceramic glazing material |
| CN103145452A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Red colorant for ceramic ink and preparation method thereof |
| CN103145447B (en) * | 2013-03-29 | 2014-07-09 | 佛山市南海万兴材料科技有限公司 | Blue inkjet ceramic pigment and preparation method thereof |
| CN103145453A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Praseodymium yellow material for ceramic ink and preparation method thereof |
| CN116947536B (en) * | 2023-09-18 | 2024-02-23 | 新明珠集团股份有限公司 | Zirconium-free ground glaze, titanium raw material opacified glazed tile and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101012341A (en) * | 2007-02-02 | 2007-08-08 | 陕西科技大学 | Method of preparing chrome-tin red colorant |
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| CN101012341A (en) * | 2007-02-02 | 2007-08-08 | 陕西科技大学 | Method of preparing chrome-tin red colorant |
Non-Patent Citations (2)
| Title |
|---|
| 郑乃章.铬锡红色料研究的现状与展望.《中国陶瓷工业》.1999,第6卷(第4期),第42－44页. |
| 铬锡红色料研究的现状与展望;郑乃章;《中国陶瓷工业》;19991231;第6卷(第4期);第42－44页 * |
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