CN112645596A - Preparation method of low-cost low-expansion ceramic zirconium-free glaze - Google Patents

Preparation method of low-cost low-expansion ceramic zirconium-free glaze Download PDF

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CN112645596A
CN112645596A CN202110070574.6A CN202110070574A CN112645596A CN 112645596 A CN112645596 A CN 112645596A CN 202110070574 A CN202110070574 A CN 202110070574A CN 112645596 A CN112645596 A CN 112645596A
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glaze
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夏光辉
王蔺森
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Jiangxi Jinweiguan Building Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating 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
    • C04B41/5022—Coating 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes

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Abstract

The invention discloses a preparation method of low-cost low-expansion ceramic zirconium-free glaze, relating to the technical field of ceramic glaze materials and comprising the following steps: mixing and ball-milling modified mica powder, quartz, spodumene, celestite and wollastonite, adding one half weight of asbestos wool, and uniformly mixing to obtain a first mixture; mixing sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, ball-milling, adding half weight of modified lignin fiber, and uniformly mixing to obtain a second mixture; adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture; and adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain the glaze. The invention has the advantages of reducing the viscosity and the expansion coefficient of the glaze, improving the bonding strength of the glaze and the ceramic blank and being not easy to crack.

Description

Preparation method of low-cost low-expansion ceramic zirconium-free glaze
Technical Field
The invention relates to the technical field of ceramic glaze, in particular to a preparation method of low-cost low-expansion ceramic zirconium-free glaze.
Background
The ceramic is made up by using natural clay and various natural minerals as main raw materials and making them pass through such processes of pulverizing, mixing, forming and calcining. Articles made of pottery clay and fired at high temperature in special kilns have been called ceramics, which are a general term for pottery and porcelain. The traditional concept of ceramics refers to all artificial industrial products which take inorganic nonmetallic minerals such as clay and the like as raw materials. It includes various products made up by using clay or clay-containing mixture through the processes of mixing, forming and calcining. Ranging from the coarsest earthenware to the finest fine ceramics and porcelain. The main raw material of the ceramic is silicate mineral (such as clay, quartz and the like) in nature, so the ceramic and the ceramic belong to the category of silicate industry with industries such as glass, cement, enamel, refractory materials and the like. The main production areas of the ceramics are Peng Ton, Jing De Town, Linling, Gao an, Fengcheng, Pingxiang, Li Chuan, Buddha mountain, Chaozhou, Dehua, Zibo, Tangshan and Bei Liu.
Ceramics are generally formed by molding and firing a mixture of clay, feldspar, quartz, and the like. In order to impart a beautiful appearance to porcelain, a layer of ceramic glaze is generally applied to porcelain, and in the case of ceramic ware, the ceramic glaze can improve the use performance, play a decorative role, and the like. The glaze material is silicate, and the glaze material applied on the ceramic ware is made up by using quartz, feldspar and clay as raw material, grinding, adding water, mixing, coating on the surface of blank body, roasting at a certain temperature and melting, and when the temperature is reduced, forming vitreous thin layer on the surface of ceramic ware. It can make the pottery increase mechanical strength, thermal stability and dielectric strength and prevent the erosion of liquid and gas, and the glaze material also has the functions of increasing the beautiful appearance of the pottery, facilitating the cleaning and brushing, preventing the porcelain from being stained by dust, etc.
Low expansion ceramics are favored for their excellent high temperature resistance, thermal shock resistance and high temperature chemical stability, and are widely used in ceramic blanks, glazes, kiln furniture microwave oven carrier plates, induction cooker panels, microwave oven liners, household heat-resistant tableware, thermocouple protection tubes, and the like. In the industrial production of ceramics, glazing is very difficult for low expansion porcelain bodies. According to the technological requirements of blank glaze combination, the thermal expansion coefficient of the glaze material is slightly less than that of the porcelain blank, otherwise, in the process of firing and cooling, the glaze material is subjected to tensile stress to generate glaze cracking. Because the thermal expansion coefficient of the ultra-low expansion ceramic body is very small, the thermal expansion coefficient is generally less than 2.0 multiplied by 10-6V. C. The coefficient of thermal expansion of the glaze needs to be smaller to adapt, and the coefficient of thermal expansion of the common glaze is 3-8 x 10-6Between/° c, the glaze of the prior art is therefore not suitable for low expansion ceramics.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provide a method for preparing low-cost and low-expansion zirconium-free glaze for ceramics.
The technical solution of the invention is as follows:
a method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 20-26 parts of spodumene, 12-16 parts of bentonite, 8-14 parts of modified mica powder, 15-20 parts of quartz, 5-10 parts of celestite, 3-7 parts of zinc oxide, 2-4 parts of barium carbonate, 1-3 parts of wollastonite, 2-4 parts of boron nitride, 1-3 parts of sepiolite powder, 2-4 parts of modified lignin fiber, 1.5-2.5 parts of sulfonated lignin, 2-4 parts of modified nano calcium carbonate, 1-3 parts of asbestos wool, 1-5 parts of plant ash and 0.5-1.5 parts of sodium hexametaphosphate;
the preparation method comprises the following steps:
s1, mixing and ball-milling the modified mica powder, quartz, spodumene, celestite and wollastonite, and then adding a part of asbestos wool to be uniformly mixed to obtain a first mixture;
s2, mixing and ball-milling sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, adding part of modified lignin fiber, and uniformly mixing to obtain a second mixture;
s3, adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture;
and S4, adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain the glaze.
In a specific embodiment of the invention, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 22-24 parts of spodumene, 13-15 parts of bentonite, 10-12 parts of modified mica powder, 16-19 parts of quartz, 6-9 parts of celestite, 4-6 parts of zinc oxide, 2.5-3.5 parts of barium carbonate, 1.5-2.5 parts of wollastonite, 2.5-3.5 parts of boron nitride, 1.5-2.5 parts of sepiolite powder, 2.5-3.5 parts of modified lignin fiber, 1.8-2.2 parts of sulfonated lignin, 2.5-3.5 parts of modified nano calcium carbonate, 1.5-2.5 parts of asbestos wool, 2-4 parts of plant ash and 0.7-1.3 parts of sodium hexametaphosphate.
In a specific embodiment of the invention, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 23 parts of spodumene, 14 parts of bentonite, 11 parts of modified mica powder, 27 parts of quartz, 8 parts of celestite, 5 parts of zinc oxide, 3 parts of barium carbonate, 2 parts of wollastonite, 3 parts of boron nitride, 2 parts of sepiolite powder, 3 parts of modified lignin fiber, 2 parts of sulfonated lignin, 3 parts of modified nano calcium carbonate, 2 parts of asbestos wool, 3 parts of plant ash and 1 part of sodium hexametaphosphate.
In a specific embodiment of the present invention, the preparation method of the modified mica powder comprises: adding feldspar powder and urea into distilled water, slowly adding 0.2mol/L titanium sulfate solution at 95-105 ℃ under the stirring condition, adjusting the pH of the solution to 5-6, raising the temperature to 50-55 ℃, reacting for 30-60 min, and finally drying at 60-65 ℃.
In a specific embodiment of the present invention, the preparation method of the modified nano calcium carbonate comprises: adding nano calcium carbonate and urea into distilled water, slowly adding 0.2mol/L titanium sulfate solution under the stirring condition of 95-105 ℃, then adding a surfactant, reacting for 30-60 min, and drying for 10-14 h at 70-75 ℃.
In a specific embodiment of the present invention, the method for preparing the modified lignin fiber comprises: the preparation method of the modified lignin fiber comprises the following steps: mixing the lignin fiber with absolute ethyl alcohol, performing ultrasonic dispersion for 10-15 min, slowly adding vinyl triethoxysilane, uniformly mixing, adjusting the pH to 7-7.5, stirring at a constant temperature of 50-55 ℃ for 15-25 h, cooling to room temperature, centrifuging, and performing vacuum drying at 70-75 ℃ to obtain the modified lignin fiber.
In a specific embodiment of the present invention, the method further includes step S5: and (5) placing the glaze obtained in the step (S4) into a storage bin for sealed storage, wherein the temperature is 20-25 ℃, the humidity is 60-65%, and the storage time is 16-24 hours.
In a specific embodiment of the present invention, the method further includes step S6: and (4) applying the glaze material treated in the step (S5) onto the ceramic green body, airing, pre-sintering the ceramic green body at 400-500 ℃ for 8-15 min, heating to 1300-1350 ℃ for firing for 20-30 min, cooling to 1050-1110 ℃ for firing for 5-10 min, and cooling to room temperature.
The invention has the beneficial effects that:
the glaze material of the invention does not add zircon or zircon sand whitening agent, has no radioactive elements, low production cost and safe use; the invention also adopts spodumene, bentonite, modified mica powder, quartz, celestite, zinc oxide, barium carbonate, wollastonite, boron nitride, sepiolite powder, modified nano calcium carbonate, plant ash, asbestos wool, modified lignin fiber and the like to be matched for use, so that Al in the glaze is enabled to be used2O3/SiO2The molar ratio is in a proper range, so that the glossiness of the glaze can be adjusted, the glaze layer is fine and smooth and bright, and the viscosity and the expansion coefficient of the glaze can be reduced; and the bonding strength of the glaze and the ceramic body can be improved, and simultaneously, the glass fiber and the asbestos wool can be melted in the sintering process, so that the sintering of the glaze is more sufficient, the density of the system is improved, and cracks are not easy to appear.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
A method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 20 parts of spodumene, 12 parts of bentonite, 8 parts of modified mica powder, 15 parts of quartz, 5 parts of celestite, 3 parts of zinc oxide, 2 parts of barium carbonate, 1 part of wollastonite, 2 parts of boron nitride, 1 part of sepiolite powder, 2 parts of modified lignin fiber, 1.5 parts of sulfonated lignin, 2 parts of modified nano calcium carbonate, 1 part of asbestos wool, 1 part of plant ash and 0.5 part of sodium hexametaphosphate;
the mica powder modification method comprises the following steps: adding 10g of mica powder into 40mL of distilled water, placing the mixture in an ice-water bath condition, adding 3mL of concentrated hydrochloric acid while stirring, and dripping 8mL of TiCl with the concentration of 2mol/L4Continuing adding 8mL of 2mol/L ammonium sulfate solution, mixing and stirring, heating the mixture to 90 ℃ in a water bath, and preserving heat for 30 min; then adjusting with ammonia waterAnd (3) filtering and washing the mixed solution until the pH value of the mixed solution is 7, and drying the mixed solution at the temperature of 80 ℃ to obtain the modified mica powder.
The modification method of the nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 8g of urea into 50mL of distilled water, slowly adding 4mL of titanium sulfate solution with the concentration of 0.2mol/L at 95 ℃ under the stirring condition until the dropwise addition is completed, adding 0.0015g of sodium dodecyl benzene sulfonate, reacting for 60min, and drying at 70 ℃ for 14h to obtain the modified nano calcium carbonate.
The method for modifying the lignin fiber comprises the following steps: mixing 1g of lignin fiber with 8mL of absolute ethyl alcohol, performing ultrasonic dispersion for 10min, slowly adding 0.8mL of vinyltriethoxysilane, uniformly mixing, adjusting the pH to 7, stirring at a constant temperature of 50 ℃ for 15h, cooling to room temperature, centrifuging, and performing vacuum drying at 70 ℃ to obtain the modified lignin fiber.
The preparation method comprises the following steps:
s1, mixing and ball-milling the modified mica powder, quartz, spodumene, celestite and wollastonite, and then adding one half weight of asbestos wool to be uniformly mixed to obtain a first mixture;
s2, mixing and ball-milling sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, adding half weight of modified lignin fiber, and uniformly mixing to obtain a second mixture;
s3, adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture;
s4, adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain a glaze;
s5, placing the glaze obtained in the step S4 into a storage bin for sealed storage, wherein the temperature is 20 ℃, the humidity is 60%, and the storage time is 16 hours;
and S6, putting the glaze material processed in the step S5 on the ceramic green body, airing, pre-burning the ceramic green body at 400 ℃ for 15min, heating to 1300 ℃ for burning for 30min, cooling to 1050 ℃ for burning for 10min, and finally cooling to room temperature.
Example 2
A method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 22 parts of spodumene, 13 parts of bentonite, 10 parts of modified mica powder, 16 parts of quartz, 6 parts of celestite, 4 parts of zinc oxide, 2.5 parts of barium carbonate, 1.5 parts of wollastonite, 2.5 parts of boron nitride, 1.5 parts of sepiolite powder, 2.5 parts of modified lignin fiber, 1.8 parts of sulfonated lignin, 2.5 parts of modified nano calcium carbonate, 1.5 parts of asbestos wool, 2 parts of plant ash and 0.7 part of sodium hexametaphosphate.
The mica powder modification method comprises the following steps: adding 10g of mica powder into 45mL of distilled water, placing the mixture in an ice-water bath condition, adding 4mL of concentrated hydrochloric acid while stirring, and dripping 9mL of TiCl with the concentration of 2mol/L4Continuing adding 9mL of 2mol/L ammonium sulfate solution, mixing and stirring, heating the mixture to 95 ℃ in a water bath, and keeping the temperature for 45 min; then ammonia water is used for adjusting the pH value of the mixed solution to 7.1, and the modified mica powder is obtained after filtration, washing and drying at 82 ℃.
The modification method of the nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 9g of urea into 50mL of distilled water, slowly adding 5mL of titanium sulfate solution with the concentration of 0.2mol/L at 100 ℃ under the stirring condition until the dropwise addition is completed, adding 0.002g of sodium dodecyl benzene sulfonate, reacting for 45min, and drying at 72 ℃ for 12h to obtain the modified nano calcium carbonate.
The method for modifying the lignin fiber comprises the following steps: mixing 1g of lignin fiber with 9mL of absolute ethanol, performing ultrasonic dispersion for 12min, slowly adding 1mL of vinyltriethoxysilane, uniformly mixing, adjusting the pH to 7.2, stirring at a constant temperature of 52 ℃ for 50h, cooling to room temperature, centrifuging, and performing vacuum drying at 72 ℃ to obtain the modified lignin fiber.
The preparation method comprises the following steps:
s1, mixing and ball-milling the modified mica powder, quartz, spodumene, celestite and wollastonite, and then adding one half weight of asbestos wool to be uniformly mixed to obtain a first mixture;
s2, mixing and ball-milling sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, adding half weight of modified lignin fiber, and uniformly mixing to obtain a second mixture;
s3, adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture;
s4, adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain a glaze;
s5, placing the glaze obtained in the step S4 into a storage bin for sealed storage, wherein the temperature is 22 ℃, the humidity is 63%, and the storage time is 20 hours;
and S6, putting the glaze material processed in the step S5 on the ceramic green body, airing, pre-sintering the ceramic green body at 450 ℃ for 12min, heating to 1325 ℃ for firing for 25min, cooling to 1080 ℃ for firing for 7min, and finally cooling to room temperature.
Example 3
A method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 23 parts of spodumene, 14 parts of bentonite, 11 parts of modified mica powder, 27 parts of quartz, 8 parts of celestite, 5 parts of zinc oxide, 3 parts of barium carbonate, 2 parts of wollastonite, 3 parts of boron nitride, 2 parts of sepiolite powder, 3 parts of modified lignin fiber, 2 parts of sulfonated lignin, 3 parts of modified nano calcium carbonate, 2 parts of asbestos wool, 3 parts of plant ash and 1 part of sodium hexametaphosphate.
The mica powder modification method comprises the following steps: adding 10g of mica powder into 50mL of distilled water, placing the mixture in an ice-water bath condition, adding 1mL of concentrated hydrochloric acid while stirring, and dripping 10mL of TiCl with the concentration of 2mol/L4Continuously adding 10mL of 2mol/L ammonium sulfate solution, mixing and stirring, heating the mixture to 90-100 ℃ in a water bath, and preserving heat for 30-60 min; then ammonia water is used for adjusting the pH value of the mixed solution to 7.2, and the modified mica powder is obtained after filtration, washing and drying at the temperature of 85 ℃.
The modification method of the nano calcium carbonate comprises the following steps: adding 1g of nano calcium carbonate and 10g of urea into 50mL of distilled water, slowly adding 6mL of titanium sulfate solution with the concentration of 0.2mol/L at 105 ℃ under the stirring condition until the dropwise addition is completed, adding 0.0025g of sodium dodecyl benzene sulfonate, reacting for 60min, and drying at 75 ℃ for 10h to obtain the modified nano calcium carbonate.
The method for modifying the lignin fiber comprises the following steps: mixing 1g of lignin fiber with 10mL of absolute ethyl alcohol, performing ultrasonic dispersion for 15min, slowly adding 1.5mL of vinyl triethoxysilane, uniformly mixing, adjusting the pH to 7.5, stirring at the constant temperature of 55 ℃ for 15h, cooling to room temperature, centrifuging, and performing vacuum drying at the temperature of 75 ℃ to obtain the modified lignin fiber.
The preparation method comprises the following steps:
s1, mixing and ball-milling the modified mica powder, quartz, spodumene, celestite and wollastonite, and then adding one half weight of asbestos wool to be uniformly mixed to obtain a first mixture;
s2, mixing and ball-milling sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, adding half weight of modified lignin fiber, and uniformly mixing to obtain a second mixture;
s3, adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture;
s4, adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain a glaze;
s5, placing the glaze obtained in the step S4 into a storage bin for sealed storage, wherein the temperature is 25 ℃, the humidity is 65%, and the storage time is 24 hours;
s6, putting the glaze processed in the step S5 on the ceramic green body, airing, pre-sintering the ceramic green body at 500 ℃ for 8min, heating to 1350 ℃ for firing for 20min, cooling to 1110 ℃ for firing for 5min, and finally cooling to room temperature.
Example 4
A method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 24 parts of spodumene, 15 parts of bentonite, 12 parts of modified mica powder, 19 parts of quartz, 9 parts of celestite, 6 parts of zinc oxide, 3.5 parts of barium carbonate, 2.5 parts of wollastonite, 3.5 parts of boron nitride, 2.5 parts of sepiolite powder, 3.5 parts of modified lignin fiber, 2.2 parts of sulfonated lignin, 3.5 parts of modified nano calcium carbonate, 2.5 parts of asbestos wool, 4 parts of plant ash and 1.3 parts of sodium hexametaphosphate.
The rest is the same as example 1.
Example 5
A method for preparing low-cost low-expansion ceramic zirconium-free glaze,
the feed is prepared from the following raw materials in parts by weight: 26 parts of spodumene, 16 parts of bentonite, 14 parts of modified mica powder, 20 parts of quartz, 10 parts of celestite, 7 parts of zinc oxide, 4 parts of barium carbonate, 3 parts of wollastonite, 4 parts of boron nitride, 3 parts of sepiolite powder, 4 parts of modified lignin fiber, 2.5 parts of sulfonated lignin, 4 parts of modified nano calcium carbonate, 3 parts of asbestos wool, 5 parts of plant ash and 1.5 parts of sodium hexametaphosphate.
The rest is the same as example 1.
Comparative example 1
Modified mica powder, wollastonite, sepiolite powder, modified lignin fiber, asbestos wool, modified nano calcium carbonate and plant ash are not added in the formula.
The rest is the same as example 1.
Comparative example 2
The manufacturing method is changed as follows: adding all the raw materials into a ball mill together for ball milling, and uniformly mixing to obtain a glaze material; and (4) applying the glaze processed in the step S5 to the ceramic green body, airing, firing the green body with the glaze at 1300 ℃ for 30min, and then cooling to room temperature.
The rest is the same as example 1.
The performance indexes of the glazes in examples 1 to 5 and comparative examples 1 to 2 were tested according to the national standard method, and the results are shown in table 1:
TABLE 1
Figure BDA0002905649090000071
Figure BDA0002905649090000081
Note: the adaptation of the blank glaze in table 1 is summarized mainly from the bonding property between the matrix and the glaze and the defects of the glaze (cracking, orange glaze and glaze shrinkage) caused by the poor adaptation of the blank glaze, and the blank glaze is superior in the absence of the defects, good in one defect and medium in the presence of two or more defects.
As can be seen from Table 1, the expansion coefficients of the ceramic antique green bricks prepared in examples 1 to 5 are 0.7 to 1.15 × 10-6The adaptability of the blank glaze is excellent at/DEG C, so that the glaze prepared in the embodiments 1-5 has low expansibility and can be decrypted and combined with a ceramic green body; comparing examples 1-5 with comparative examples 1-2, it can be seen that the expansion coefficient of the ceramic antique green bricks prepared in examples 1-5 is obviously lower than that of comparative example 1 (different formula) and comparative example 2 (different preparation method), and the adaptability of the green glaze is better than that of comparative example 1 (different formula) and comparative example 2 (different preparation method), so that the glaze with low expansion and excellent adaptability of the green glaze can be obtained by selecting specific raw materials and adopting a specific process.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.

Claims (8)

1. A method for preparing low-cost low-expansion ceramic zirconium-free glaze is characterized in that,
the feed is prepared from the following raw materials in parts by weight: 20-26 parts of spodumene, 12-16 parts of bentonite, 8-14 parts of modified mica powder, 15-20 parts of quartz, 5-10 parts of celestite, 3-7 parts of zinc oxide, 2-4 parts of barium carbonate, 1-3 parts of wollastonite, 2-4 parts of boron nitride, 1-3 parts of sepiolite powder, 2-4 parts of modified lignin fiber, 1.5-2.5 parts of sulfonated lignin, 2-4 parts of modified nano calcium carbonate, 1-3 parts of asbestos wool, 1-5 parts of plant ash and 0.5-1.5 parts of sodium hexametaphosphate;
the preparation method comprises the following steps:
s1, mixing and ball-milling the modified mica powder, quartz, spodumene, celestite and wollastonite, and then adding a part of asbestos wool to be uniformly mixed to obtain a first mixture;
s2, mixing and ball-milling sepiolite powder, bentonite, boron nitride, barium carbonate and zinc oxide, adding part of modified lignin fiber, and uniformly mixing to obtain a second mixture;
s3, adding sodium hexametaphosphate, plant ash and the rest asbestos wool into the first mixture and the second mixture, and uniformly mixing to obtain a third mixture;
and S4, adding the modified nano calcium carbonate and the rest of the modified lignin fiber into the third mixture, and uniformly mixing to obtain the glaze.
2. The preparation method of the low-cost low-expansion ceramic zirconium-free glaze according to claim 1, characterized by comprising the following raw materials in parts by weight: 22-24 parts of spodumene, 13-15 parts of bentonite, 10-12 parts of modified mica powder, 16-19 parts of quartz, 6-9 parts of celestite, 4-6 parts of zinc oxide, 2.5-3.5 parts of barium carbonate, 1.5-2.5 parts of wollastonite, 2.5-3.5 parts of boron nitride, 1.5-2.5 parts of sepiolite powder, 2.5-3.5 parts of modified lignin fiber, 1.8-2.2 parts of sulfonated lignin, 2.5-3.5 parts of modified nano calcium carbonate, 1.5-2.5 parts of asbestos wool, 2-4 parts of plant ash and 0.7-1.3 parts of sodium hexametaphosphate.
3. The preparation method of the low-cost low-expansion ceramic zirconium-free glaze according to claim 1, characterized by comprising the following raw materials in parts by weight: 23 parts of spodumene, 14 parts of bentonite, 11 parts of modified mica powder, 27 parts of quartz, 8 parts of celestite, 5 parts of zinc oxide, 3 parts of barium carbonate, 2 parts of wollastonite, 3 parts of boron nitride, 2 parts of sepiolite powder, 3 parts of modified lignin fiber, 2 parts of sulfonated lignin, 3 parts of modified nano calcium carbonate, 2 parts of asbestos wool, 3 parts of plant ash and 1 part of sodium hexametaphosphate.
4. The method for preparing the low-cost and low-expansion ceramic zirconium-free glaze according to claim 1, wherein the method for preparing the modified mica powder comprises the following steps: adding mica powder into distilled water, placing in ice water bath, adding concentrated hydrochloric acid while stirring, and dripping TiCl4Continuously adding the ammonium sulfate solution into the solution, mixing and stirring, heating the mixture to 95-105 ℃ in a water bath, and preserving heat for 30-60 min; then dropwise adding the prepared ammonia water solution until the pH value is 7.2-7.5, filtering, washing at 70-80 DEG CAnd drying to obtain the modified mica powder.
5. The method for preparing the zirconium-free glaze with low cost and low expansion as claimed in claim 1, wherein the method for preparing the modified nano calcium carbonate comprises the following steps: adding nano calcium carbonate and urea into distilled water, slowly adding 0.2mol/L titanium sulfate solution under the stirring condition of 95-105 ℃, then adding a surfactant, reacting for 30-60 min, and drying for 10-14 h at 70-75 ℃.
6. The method for preparing the zirconium-free glaze with low cost and low expansion as claimed in claim 1, wherein the method for preparing the modified lignin fiber comprises the following steps: the preparation method of the modified lignin fiber comprises the following steps: mixing the lignin fiber with absolute ethyl alcohol, performing ultrasonic dispersion for 10-15 min, slowly adding vinyl triethoxysilane, uniformly mixing, adjusting the pH to 7-7.5, stirring at a constant temperature of 50-55 ℃ for 15-25 h, cooling to room temperature, centrifuging, and performing vacuum drying at 70-75 ℃ to obtain the modified lignin fiber.
7. The method for preparing the zirconium-free glaze with low cost and low expansion for ceramics according to claim 1, further comprising the step of S5: and (5) placing the glaze obtained in the step (S4) into a storage bin for sealed storage, wherein the temperature is 20-25 ℃, the humidity is 60-65%, and the storage time is 16-24 hours.
8. The method for preparing the zirconium-free glaze with low cost and low expansion for ceramics according to claim 7, further comprising the step of S6: and (4) applying the glaze material treated in the step (S5) onto the ceramic green body, airing, pre-sintering the ceramic green body at 400-500 ℃ for 8-15 min, heating to 1300-1350 ℃ for firing for 20-30 min, cooling to 1050-1110 ℃ for firing for 5-10 min, and cooling to room temperature.
CN202110070574.6A 2021-01-19 2021-01-19 Preparation method of low-cost low-expansion ceramic zirconium-free glaze Pending CN112645596A (en)

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