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CN107459261B - Low-temperature orange pigment for ceramic glaze and preparation method thereof - Google Patents

Low-temperature orange pigment for ceramic glaze and preparation method thereof Download PDF

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Publication number
CN107459261B
CN107459261B CN201710704845.2A CN201710704845A CN107459261B CN 107459261 B CN107459261 B CN 107459261B CN 201710704845 A CN201710704845 A CN 201710704845A CN 107459261 B CN107459261 B CN 107459261B
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low
temperature
ceramic glaze
ceramic
orange pigment
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CN107459261A (en
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李桂贤
刁龙海
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Fujian Dehua Grangtop Ceramic Co Ltd
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Fujian Dehua Grangtop Ceramic Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02Frit compositions, i.e. in a powdered or comminuted form
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/86Glazes; Cold glazes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Glass Compositions (AREA)

Abstract

The invention particularly relates to a low-temperature orange pigment for ceramic glaze and a preparation method thereof, belonging to the technical field of ceramic pigments. The low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 65-67% of german Geder, 18-20% of low-temperature frit, 11-12.5% of Longyan kaolin and the balance of magnesium chloride. The composite material is prepared by mixing, calcining, quenching and ball milling, has simple production process and low requirement on equipment, is suitable for industrial production, saves energy, reduces emission and is environment-friendly. The pigment has stable color, small color difference change, full tone and bright texture, and consistent color with artificially synthesized materials, is suitable for daily decorative ceramics, building ceramics and the like, and can be quickly fired at 1060-1150 ℃.

Description

Low-temperature orange pigment for ceramic glaze and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic pigments, and particularly relates to a low-temperature orange pigment for ceramic glaze and a preparation method thereof.
Background
The ceramic pigment is also called pigment or color material, and is a special color material for powdered colored ceramics prepared from a color base and a fusing agent or an additive.
In the prior art, the ceramic pigment is generally prepared by mixing a coloring metal oxide or a chemical raw material with other additives. In a patent with the application number of 201510676599.5 and the name of 'praseodymium zirconium yellow ceramic pigment with small particle size and a preparation method thereof', praseodymium oxide and zirconium oxide are used as chromophore, and silicon dioxide is used as a fusing agent to prepare the ceramic pigment, but the praseodymium oxide and the zirconium oxide are expensive and high in cost, and the natural price of the prepared pigment is not low. In the patent with application number 201410543206.9 entitled "neodymium disilicate high-temperature ceramic pigment and preparation method thereof", the preparation method comprises the following steps: (1) adding neodymium nitrate and ethyl orthosilicate into the water/alcohol mixed solution, uniformly stirring, adding polyethylene glycol, and stirring and dispersing to obtain sol containing neodymium and silicon; (2) dropwise adding a precipitating agent into the obtained neodymium-and-silicon-containing sol until the pH value of the sol is 8.5-9.0 to obtain a precipitation solution; (3) standing and aging the obtained precipitation solution, then performing centrifugal treatment, and then washing the centrifugal solid precipitate with absolute ethyl alcohol to obtain a precipitate; (4) and (3) drying the obtained precipitate in a forced air drying box, and then calcining the dried precipitate at high temperature to obtain the catalyst. The method is carried out with sol preparation, precipitant dripping, centrifugation and other treatments before high-temperature calcination, and has complex operation, and a certain amount of chemical reagent is also used, which has influence on the environment.
Therefore, the invention aims to provide the low-temperature orange pigment for the ceramic glaze, which has the advantages of cheap and easily-obtained preparation raw materials, low cost, simple production process, stable color, full hue, bright texture and consistent color with artificially synthesized materials.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a low-temperature orange pigment for ceramic glaze and a preparation method thereof, the pigment has the advantages of cheap and easily-obtained preparation raw materials, simple production process, stable color, small color difference change, full tone and bright texture, consistent color with artificially synthesized materials, suitability for daily decorative ceramics and the like, and capability of being quickly fired at 1060-1150 ℃.
The technical scheme adopted by the invention is as follows:
the low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 65-67% of german Geder, 18-20% of low-temperature frit, 11-12.5% of Longyan kaolin and the balance of magnesium chloride.
Further, the method comprises the following raw materials in percentage by mass: 66.5% of german Geder, 20% of low-temperature frit, 12% of Longyan kaolin and 1.5% of magnesium chloride.
Furthermore, the softening point of the low-temperature frit is not higher than 700 ℃, and the firing temperature is 900-1080 ℃.
The preparation method of the low-temperature orange pigment for the ceramic glaze comprises the following steps:
1) weighing the raw material components according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 8-12h, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 1-3 min;
4) and after quenching, putting the mixture into a ball mill for ball milling for 48 to 72 hours, and then sieving the mixture through a 200-plus-400-mesh sieve to obtain the low-temperature orange pigment for the ceramic glaze.
Furthermore, the raw material components are firstly crushed and sieved by a 200-mesh sieve before mixing in the step 1), so that subsequent uniform mixing is facilitated.
Further, the calcination time in step 2) was 10 h.
Further, after quenching in the step 4), putting the mixture into a ball mill for ball milling for 72 hours, and then sieving the mixture through a 250-mesh sieve.
The invention has the beneficial effects that:
firstly, the orange pigment prepared by the invention has stable color, small color difference change, full tone and bright texture, consistent color with artificially synthesized materials, is suitable for daily decorative ceramics, building ceramics and the like, and can be quickly fired at 1060-1150 ℃;
secondly, the invention breaks through the conventional method of artificially synthesizing colored metal oxide or chemical raw materials, but uses cheap and easily obtained raw materials such as German Geder, low-temperature frit, Longyan kaolin and magnesium chloride, prepares the pigment through a plurality of simple procedures of mixing, calcining, quenching and ball milling, has low requirement on equipment, is suitable for industrial production, saves energy and reduces emission, and is environment-friendly. The german clay is high-quality porcelain clay since ancient times due to special geographical positions, and the Longyan kaolin contains less than 0.3 percent of iron and less than 0.02 percent of titanium and contains a certain amount of low-temperature solvent elements (Li)2O) and the low-temperature frit generate a synergistic effect, so that the pigment cannot have the problems of instability and large color difference due to the factors of fluctuation of the quality of raw materials, narrow formula proportion range, temperature difference influence and the like, but is fine and elegant, and the stability is enhanced by adding the magnesium chloride, and meanwhile, the light sensation texture is enhanced.
Detailed Description
The present invention is described in further detail below with reference to examples, but the present invention should not be construed as being limited thereto. The raw materials used in the present invention may be commercially available unless otherwise specified.
Example 1
The low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 65% of german Geder soil, 18% of low-temperature frit, 11% of Longyan kaolin and 6% of magnesium chloride, wherein the low-temperature frit is a code LK7340 low-temperature frit produced by Zibofloxacin ceramic color glaze Co., Ltd, the softening point is 700 ℃, and the firing temperature is 1000-1080 ℃.
The preparation method of the low-temperature orange pigment for the ceramic glaze comprises the following steps:
1) weighing the raw material components according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 8 hours, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 1 min;
4) quenching, ball milling in a ball mill for 60h, and sieving with a 200-mesh sieve.
Example 2
The low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 66.5 percent of german Geder soil, 20 percent of low-temperature frit, 12 percent of Longyan kaolin and 1.5 percent of magnesium chloride, wherein the low-temperature frit is LK7340 low-temperature frit produced by Zibofloxacin ceramic color glaze Co., Ltd, the softening point is 700 ℃, and the firing temperature is 1000-1080 ℃.
The preparation method of the low-temperature orange pigment for the ceramic glaze comprises the following steps:
1) crushing and sieving the raw material components, weighing according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 12 hours, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 2 min;
4) and after quenching, putting the mixture into a ball mill for ball milling for 72 hours, and then sieving the mixture through a 300-mesh sieve to obtain the product.
Example 3
The low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 66% of Dehuagaide soil, 19% of low-temperature frit, 11.5% of Longyan kaolin and 3.5% of magnesium chloride, wherein the low-temperature frit is Zibo cis-Tai ceramic type T-908 low-temperature frit, the softening point is 600 ℃, and the firing temperature is 1000-1080 ℃.
The preparation method of the low-temperature orange pigment for the ceramic glaze comprises the following steps:
1) crushing and sieving the raw material components, weighing according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 12 hours, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 3 min;
4) and after quenching, putting the mixture into a ball mill for ball milling for 72 hours, and then sieving the mixture through a 200-mesh sieve to obtain the product.
Example 4
The low-temperature orange pigment for the ceramic glaze comprises the following raw materials in percentage by mass: 67% of Dehua Gede soil, 20% of low-temperature frit, 12.5% of Longyan kaolin and 0.5% of magnesium chloride, wherein the low-temperature frit is a Zibo cis-Tai ceramic low-temperature frit with the model number of T-908, the softening point is 600 ℃, and the firing temperature is 1000-1080 ℃.
The preparation method of the low-temperature orange pigment for the ceramic glaze comprises the following steps:
1) crushing and sieving the raw material components, weighing according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 10 hours, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 2 min;
4) and after quenching, putting the mixture into a ball mill for ball milling for 72 hours, and then sieving the mixture through a 250-mesh sieve to obtain the product.
Performance testing
The orange colorants prepared in inventive examples 1-4 were tested for performance and the results are shown in the following table:
test items Example 1 Example 2 Example 3 Example 4
Firing temperature 1120℃ 1150℃ 1100℃ 1060℃
Color difference 0.1 0.05 0.05 0.05
Lightness difference 0.15 0.2 -0.05 0.05
Difference in chroma 0.1 0.05 0.05 0.1
Wherein the color difference measurement is performed according to the Lab principle of the CIE color space using a color difference tester SP 62.
As can be seen from the table, the orange pigment prepared by the invention can be quickly fired at 1060-1150 ℃, has stable color, small color difference change, full color tone and bright texture. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. The low-temperature orange pigment for the ceramic glaze is characterized by comprising the following raw materials in percentage by mass: 65-67% of german Geder, 18-20% of low-temperature frit, 11-12.5% of Longyan kaolin and the balance of magnesium chloride.
2. The low-temperature orange pigment for the ceramic glaze according to claim 1, which is characterized by comprising the following raw materials in percentage by mass: 66.5% of german Geder, 20% of low-temperature frit, 12% of Longyan kaolin and 1.5% of magnesium chloride.
3. The low-temperature orange-yellow colorant for ceramic glazes according to claim 1 or 2, characterized in that the softening point of the low-temperature frit is not higher than 700 ℃ and the firing temperature is 900 ℃ to 1080 ℃.
4. The method for making a low temperature orange colorant for ceramic glazes of claim 1, characterized by comprising the steps of:
1) weighing the raw material components according to the proportion, uniformly mixing, soaking for 24h, and dehydrating;
2) calcining the material obtained in the step 1) for 8-12h, wherein the calcining temperature is controlled to be 1250-1270 ℃;
3) pouring the calcined material into water to quench for 1-3 min;
4) and after quenching, putting the mixture into a ball mill for ball milling for 48 to 72 hours, and then sieving the mixture through a 200-plus-400-mesh sieve to obtain the low-temperature orange pigment for the ceramic glaze.
5. The method for preparing a low-temperature orange pigment for ceramic glaze according to claim 4, wherein the raw material components are crushed and sieved with a 200-mesh sieve before being mixed in the step 1).
6. The method for preparing a low-temperature orange colorant for ceramic glazes according to claim 4, characterized in that the calcination time in step 2) is 10 hours.
7. The method for preparing a low-temperature orange pigment for ceramic glaze according to claim 4, wherein the step 4) is carried out by placing the cooled ceramic glaze into a ball mill for ball milling for 72h, and then sieving the ceramic glaze with a 250-mesh sieve.
CN201710704845.2A 2017-08-17 2017-08-17 Low-temperature orange pigment for ceramic glaze and preparation method thereof Active CN107459261B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101759440A (en) * 2009-12-18 2010-06-30 深圳市永丰源实业有限公司 Lead-free ceramic glaze and preparation process thereof
CN101759441B (en) * 2009-12-31 2013-03-13 深圳市永丰源实业有限公司 Ceramic glaze and preparation process thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL9200293A (en) * 1992-02-18 1993-09-16 Colorsil Bv Doped zirconium blend silicate, process for its preparation, and products containing such or similarly prepared pigments.

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101759440A (en) * 2009-12-18 2010-06-30 深圳市永丰源实业有限公司 Lead-free ceramic glaze and preparation process thereof
CN101759441B (en) * 2009-12-31 2013-03-13 深圳市永丰源实业有限公司 Ceramic glaze and preparation process thereof

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