CN102515533A - Alkali silicate glass frit, zirconium frit opaque glaze, zirconium raw material opaque glaze and preparation methods of the zirconium frit opaque glaze and the zirconium raw material opaque glaze - Google Patents
Alkali silicate glass frit, zirconium frit opaque glaze, zirconium raw material opaque glaze and preparation methods of the zirconium frit opaque glaze and the zirconium raw material opaque glaze Download PDFInfo
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Abstract
The invention discloses an alkali silicate glass frit, a zirconium frit opaque glaze, a zirconium raw material opaque glaze, and preparation methods of the zirconium frit opaque glaze and the zirconium raw material opaque glaze. The preparation methods are ceramic glazing methods. Main raw materials of the zirconium frit opaque glaze comprise frits prepared from waste silica gel and sodium carbonate, wherein utilization amounts of waste silica gel and sodium carbonate satisfy a SiO2-Na2O mole ratio of (2 to 3): 1. Waste silica gel and other raw materials are directly prepared into pulp and then are sintered into the zirconium raw material opaque glaze. The zirconium frit opaque glaze and the zirconium raw material opaque glaze are prepared from raw materials of zirconium-containing waste silica gel (which is short for waste silica gel), and residual zirconium of the raw materials is utilized as an opacifier, and thus the problems of waste silica gel storage and environmental pollution are solved. The types of the used raw materials are reduced. An opaque glaze production cost is reduced. In preparation, waste silica gel can be directly used without physical and chemical treatment. The zirconium frit opaque glaze and the zirconium raw material opaque glaze are convenient for industrial application, and have performances satisfying general requirements.
Description
Technical field
The present invention relates to a kind of alkali silicate glass frit, opaque glaze and preparation method thereof, be specifically related to a kind of alkali silicate glass frit, zirconium opaque glaze and preparation method thereof, belong to technical field of inorganic nonmetallic materials.
Background technology
Glass frit can be used for producing opaque glaze, is that the alkali silicate glass frit of staple is still produced water glass (popular name: raw material bubble flower alkali) with sodium oxide and silicon-dioxide.Opaque glaze is widely used in pottery, enamelled and decorates, and the root of milkiness is owing to produced second phase different with the host glass specific refractory power because of phase-splitting or crystallization in vitreous glaze, causes thereby mostly occur therein when causing light through glaze repeatedly to reflect.Zirconium opaque glaze is one of widely used opaque glaze, the history of the existing last 100 years of its research.Zirconium opaque glaze has the whiteness height, opaque effect is good, covering power is strong, can reduce base with the requirement of raw material and technology controlling and process, advantage such as the milkiness effect is stable, insensitive to atmosphere, cost is lower, can be used for the production of sanitary china, ornamental brick and enamel product.
Usually, utilize zircon sand, zirconium silicate or zirconium white to prepare zirconium opaque glaze for opacifying agent.Opaque mechanism is that the zirconium compounds particulate through remaining in the glaze or recrystallize produces milkiness.Prepare process at zironium glaze, add zirconium opacifying agent, or directly zirconium opacifying agent is prepared burden with other raw material after separate out again behind the high-temperature digestion and contain zirconium crystalline form and realize opaque effect through mill in frit.Zirconium opacifying agent fusing point is high, and the firing temperature of glaze is higher.No matter with which kind of zirconium opacifying agent, last acting have only zircon and two kinds of crystalline phases of baddeleyite.Zircon sand or zirconium white are that opacifying agent occupies larger proportion in the cost of zirconium opaque glaze.In addition; The zirconium opaque glaze batching is formed complicated, and more use contains the raw material of lithium or boron, in patent CN200710139659.5 (middle temperature high-white zirconium-lithium slurry opaque glaze and working method thereof); Except that using 10～15% zirconium English powder, also need add 12～15% lithium porcelain stones; Except that using 13～18% zirconium silicates, also need add 15～25% boric acid among the patent CN201010559507.2 (a kind of piezoelectric ceramics atomizing piece is with white opaque glaze and preparation method thereof).Raw material type is many, not only increases raw materials cost, also increases raw material and handles, deposits and the process procedure cost.
Zirconic discarded silica gel (hereinafter to be referred as " useless silica gel ") is derived from mineral and refines the solid waste that produces behind the zirconium products such as zirconium white or zirconium oxychloride; Its staple is silicon-dioxide and ZIRCONIUM DIOXIDE 99.5 (5-12%); The former is one of staple of alkali silicate glass frit and zirconium opaque glaze, and the latter can be used as the opacifying agent of opaque glaze.In addition, also contain a spot of calcium, aluminium in the discarded silica gel, they still are the beneficiating ingredient of zirconium opaque glaze.At present, the bright rare report of the opaque glaze that zirconic discarded silica gel is raw material if it is made into opaque glaze as opacifying agent, can reduce cost greatly, and is very meaningful to the industrial applications of zirconium opacifying agent.
Summary of the invention
The invention provides a kind of is the alkali silicate glass frit of raw material with useless silica gel; This frit tradition to be used for the alkali silicate glass frit that water glass produces meltable, reduce temperature of fusion 20-150 ℃ approximately, in addition; The gained glass frit will help to tackify and intensity because of introducing zirconium.
In addition, to the existing shortcoming that the zirconium opaque glaze raw material is many, production cost is high, the present invention also provides two kinds of zirconium opaque glazes; They all (are called for short useless silica gel with zirconic discarded silica gel; Be raw material down together), utilize wherein residual zirconium to be opacifying agent, promptly solved useless silica gel to deposit and environmental pollution problem; Reduce raw material again and use kind, reduced the production cost of opaque glaze.
Further, the present invention also provides the preparation method of zirconium opaque glaze, and its preparation raw material is few, and useless silica gel need not physics, chemical treatment can directly be used, and is convenient to industrial applications.
Main purpose of the present invention is industrial solid castoff---zirconic discarded silica gel some application in the big production of actual industrialization that produce in research zirconium white or the zirconium oxychloride production process; Research shows; With useless silica gel is that raw material can be processed alkali silicate glass frit, zirconium opaque glaze; Turn waste into wealth, promptly protected environment to reduce production cost again.
Its concrete technical scheme is following:
A kind of alkali silicate glass frit is characterized in that: raw material comprises useless silica gel and soda ash, and the consumption of wherein useless silica gel and soda ash satisfies the SiO that introduces
2And Na
2The mol ratio of O is 2-3:1.
Above-mentioned gained frit also can directly be used to produce the raw material of water glass (being commonly called as bubble flower alkali), and the temperature of fusion of general frit is between 1250-1280 ℃.
The invention provides a kind of zirconium frit opaque glaze; Replaced traditional zirconium silicate, zircon sand or zirconium white opacifying agent with useless silica gel and prepared zirconium opaque glaze, raw material comprises: a) frit, b) clay; C) at least a in albite, Wingdale and the fluorite; Wherein, frit is formed by useless silica gel and soda ash, and the consumption of useless silica gel and soda ash satisfies the SiO that introduces
2And Na
2The mol ratio of O is 2-3:1, and the consumption of clay is 1% of a frit quality, and the consumption of c raw material is 5% of a frit quality.
In the above-mentioned zirconium frit opaque glaze, said useless silica gel mainly is made up of silicon-dioxide and zirconium white, and wherein, zirconic content is the 5-12wt% of useless silica gel.
Above-mentioned zirconium frit opaque glaze preparation method is characterized in that, may further comprise the steps:
(1) gets useless silica gel and soda ash in proportion, mix, be heated to 1250 ~ 1280 ℃ and make its fusing;
(2) the glass metal shrend after will melting, filter are done, oven dry, frit;
(3) frit is mixed with other raw material (refer in above-mentioned raw material b clay and raw material c albite, Wingdale and the fluorite at least a), carry out ball milling slurrying;
(4) the gained slurry is transferred to suitable concentration, adopts and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
(5) ceramic body after the glazing burns till under 1000 ℃, insulation 1h, and furnace cooling gets goods.
When ball milling, the amount of used abrading-ball, water and the mass ratio of raw material adopt the general ratio in this area to get final product, and those skilled in the art can select from prior art.
Above-mentioned fritted glaze as opacifying agent, also contains a large amount of silicon-dioxide in the useless simultaneously silica gel, for opaque glaze provides raw material with useless silica gel.In the present invention's prescription, raw material type is few, and cost is low; The performance of gained glaze satisfies the demand of general sanitary china, ornamental brick, in addition, because zirconic discarded silica gel is amorphous state; And zirconium is distribution uniform therein, so it can make as zirconium opacifying agent, and glaze is meltable, composition is even.
The present invention also provides a kind of zirconium opaque enamel of raw material, it is characterized in that comprising following raw materials by weight percent:
Useless silica gel 32-56%
Silica sand 0-23%
Feldspar 16-41%
Wingdale 2-12%
Aluminum oxide 0-8.4%
Zinc oxide 0-4.3%
Fluorite 2.9-4.8%
Kaolin 0-17.5%
Natural manganese dioxide 0-1%.
In the above-mentioned zirconium opaque enamel of raw material, said useless silica gel mainly is made up of silicon-dioxide and zirconium white, and wherein the content of silicon oxide is the 5-12wt% of useless silica gel.
The present invention also provides with this opaque enamel of raw material and has carried out ceramic glazing method, it is characterized in that, may further comprise the steps:
(1), carries out ball milling slurrying with each raw materials mix;
(2) the gained slurry is transferred to suitable concentration, adopts and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
(3) with the body drying after the glazing, burn till at 1200 ~ 1280 ℃ then, insulation 0.5-1h, furnace cooling gets goods.
When ball milling, the amount of used abrading-ball, water and the mass ratio of raw material adopt the general ratio in this area to get final product, and those skilled in the art can select from prior art.
Above-mentioned raw glaze is a raw material with the discarded silica gel of undressed zirconic silicon-dioxide; Reduced raw material type; The particularly use of expensive raw material; Alleviated useless silica gel aftertreatment burden, promptly utilized trade waste to reduce the production cost of zirconium opaque glaze again, good environment and economic results in society have been arranged.In addition; Because zirconic discarded silica gel is amorphous state, and zirconium distribution uniform therein, so it can make as zirconium opacifying agent, and glaze is meltable, composition is even; The opaque glaze performance of gained can satisfy general requirement, can be used for the decoration of general ornamental brick, bottle, sanitary china, enamel etc.
Embodiment
Through specific embodiment the present invention is further set forth below, should be understood that, following explanation only is in order to explain the present invention, its content not to be limited.Following raw material is formed if there is not explanation, all is weight percentage.
Embodiment 1
With useless silica gel, soda ash is that raw material is processed frit, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 75:25, i.e. 3:1.The method for preparing frit is following:
1, gets useless silica gel and soda ash in proportion, mix, in electric furnace or kiln, be heated to 1280 ℃, make its fusing;
2, the glass metal shrend after will melting, filter are done, 120 ℃ of oven dry, frit.The gained frit can directly be used to produce the raw material of water glass (being commonly called as bubble flower alkali), also can be used as the raw material of opaque glaze.
Embodiment 2
With useless silica gel, soda ash is that raw material is processed frit, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 67:33, except useless silica gel and soda ash be heated to melt under 1250 ℃, other prepare the step such as the embodiment 1 of frits.
Embodiment 3
With useless silica gel, soda ash, clay and albite is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 75:25, i.e. 3:1, and the consumption of clay is 1% of a frit total amount, the consumption of albite is 5% of useless silica gel and soda ash total amount.Useless silica gel and soda ash add with the form of frit, and the method for preparing fritted glaze is following:
1, gets useless silica gel and soda ash in proportion, mix, in electric furnace or kiln, be heated to 1280 ℃, make its fusing;
2, the glass metal shrend after will melting, filter are done, 120 ℃ of oven dry, frit;
3, frit is mixed with clay, albite, carry out ball milling slurrying (material: water: the ball mass ratio is 1:0.7:1.5);
4, adopt and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
5, the ceramic body after the glazing burns till insulation 1h under 1000 ℃, and furnace cooling gets goods.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 4
Except that albite replaced with the lightweight Wingdale, other were like embodiment 3.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 5
Except that albite replaced with fluorite, other were like embodiment 3.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 6
With useless silica gel, soda ash, clay and albite, lightweight Wingdale and fluorite is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 75:25, i.e. 3:1, and the consumption of clay is 1% of a frit total amount, and the consumption of albite is 1.5% of a frit, and the consumption of lightweight Wingdale is 3.0% of a frit, and the consumption of fluorite is 0.5% of a frit.Useless silica gel and soda ash add preparation method such as embodiment 3 with the form of frit.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 7
With useless silica gel, soda ash, clay, lightweight Wingdale and fluorite is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 67:33, and the consumption of clay is 1% of useless silica gel and soda ash total amount, and the consumption of lightweight Wingdale is 1% of a frit, and the consumption of fluorite is 4% of a frit, and useless silica gel and soda ash add with the form of frit.Except useless silica gel and soda ash be heated to melt under 1250 ℃, prepare the method embodiment 3 of fritted glaze.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 8
The consumption that removes the lightweight Wingdale is 4% of a frit, and the consumption of fluorite is 1% of a frit, and other are like embodiment 7.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 9
With useless silica gel, soda ash, clay, albite and lightweight Wingdale is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 67:33, and the consumption of clay is 1% of useless silica gel and soda ash total amount, and the consumption of albite is 2.5% of useless silica gel and soda ash total amount, and the consumption of lightweight Wingdale is 2.5% of useless silica gel and soda ash total amount.Useless silica gel and soda ash add with the form of frit, and the method for preparing fritted glaze is following:
1, gets useless silica gel and soda ash in proportion, mix, in electric furnace or kiln, be heated to 1250 ℃, it is dissolved;
2, the glass metal shrend after will melting, filter are done, 120 ℃ of oven dry, frit;
3, frit is mixed with clay, albite, lightweight Wingdale, carry out ball milling slurrying (material: water: the ball mass ratio is 1:0.7:1.5);
4, adopt and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
5, the ceramic body after the glazing burns till insulation 1h under 1000 ° of C, and furnace cooling gets goods.Gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 10
With useless silica gel, soda ash, clay, fluorite and lightweight Wingdale is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 75:25; Be 3:1, and the consumption of clay is 1% of useless silica gel and soda ash total amount, the consumption of fluorite is 2.5% of useless silica gel and soda ash total amount; The consumption of lightweight Wingdale is 2.5% of useless silica gel and soda ash total amount, and useless silica gel and soda ash add with the form of frit.Except useless silica gel and soda ash be heated to melt under 1280 ℃, prepare the method such as the embodiment 6 of fritted glaze, gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 11
With useless silica gel, soda ash, clay, fluorite and albite is that raw material is processed opaque glaze, contains the zirconium white of 5-12wt% in the wherein useless silica gel, and all the other are silicon-dioxide.In raw material, the consumption of useless silica gel and soda ash satisfies introduces SiO
2And Na
2The mol ratio of O is 75:25; Be 3:1, and the consumption of clay is 1% of useless silica gel and soda ash total amount, the consumption of fluorite is 2.5% of useless silica gel and soda ash total amount; The consumption of albite is 2.5% of useless silica gel and soda ash total amount, and useless silica gel and soda ash add with the form of frit.Except useless silica gel and soda ash be heated to melt under 1280 ℃, prepare the method such as the embodiment 6 of fritted glaze, gained glaze visual appearance can satisfy the general requirement of common milkiness ceramic such as ornamental brick etc.
Embodiment 12
With useless silica gel 32.2%, silica sand 22.3%, feldspar 16%, Wingdale 12.2%, aluminum oxide 8.4%, zinc oxide 4.2%, fluorite 4.7% is raw material, and each raw material sum is 100%, and glaze of the present invention need not frit, can directly process raw glaze, and its method for making is following:
1,, carries out ball milling slurrying (material: water: the mass ratio of ball is 1:1.2:2) with each raw materials mix;
2, adopt and to soak glaze, be coated with glaze or glaze spraying mode the ceramic body glazing;
3, with the body drying after the glazing, burn till 0.5-1h at 1200 ~ 1280 ℃ then, furnace cooling gets goods.
Embodiment 13
With useless silica gel 32.6%, silica sand 7.1%, feldspar 24.3%, Wingdale 8.5%, kaolin 17.5%, zinc oxide 4.2%, fluorite 4.8%, lightweight MgO 1% is raw material, and each raw material sum is 100%, preparation method such as embodiment 12.
Embodiment 14
With useless silica gel 49%, feldspar 24.5%, Wingdale 8.4%, kaolin 4.2%, zinc oxide 4.3%, fluorite 4.8%, aluminum oxide 3.8%, MgO 1% is raw material, and each raw material sum is 100%, and the preparation method is:
1,, carries out ball milling slurrying (material: water: the mass ratio of ball is 1:1.2:2) with each raw materials mix;
2, adopt and to soak glaze, be coated with glaze or glaze spraying mode the ceramic body glazing;
3, with the body drying after the glazing, burn till 0.5h at 1250 ℃ then, furnace cooling gets goods.
Embodiment 15
With useless silica gel 56%, feldspar 22.9%, Wingdale 2%, kaolin 10.5%, fluorite 2.9%, aluminum oxide 5.2%, MgO 0.5% is raw material, and each raw material sum is 100%, preparation method such as embodiment 14.
Embodiment 16
With useless silica gel 32%, silica sand 17%, feldspar 41%, Wingdale 5%, fluorite 4%, lightweight MgO1% is raw material, and each raw material sum is 100%, preparation method such as embodiment 12.
In the foregoing description, whiteness, glossiness and the density of three of gained glaze appearance are as shown in table 1 below among the embodiment 12-14, and the performance of the glaze appearance of embodiment 15,16 is close with embodiment 14.The prepared glaze performance of embodiment 12-16 satisfies general requirement, can be used on the utensils such as bottle, sanitary china.
Claims (8)
1. alkali silicate glass frit is characterized in that: raw material comprises useless silica gel and soda ash, and the consumption of wherein useless silica gel and soda ash satisfies the SiO of introducing
2And Na
2The mol ratio of O is 2-3:1.
2. alkali silicate glass frit according to claim 1 is characterized in that: said useless silica gel mainly is made up of silicon-dioxide and zirconium white, and wherein, zirconic content is the 5-12wt% of useless silica gel.
3. zirconium frit opaque glaze is characterized in that raw material comprises: a) frit, and b) clay, c) at least a in albite, Wingdale and the fluorite, wherein, frit is formed by useless silica gel and soda ash, and the consumption of useless silica gel and soda ash satisfies the SiO of introducing
2And Na
2The mol ratio of O is 2-3:1, and the consumption of clay is 1% of a frit quality, and the consumption of c raw material is 5% of a frit quality.
4. zirconium frit opaque glaze according to claim 3 is characterized in that: said useless silica gel mainly is made up of silicon-dioxide and zirconium white, and wherein, zirconic content is the 5-12wt% of useless silica gel.
5. the preparation method of the described zirconium frit of claim 3 opaque glaze is characterized in that, may further comprise the steps:
(1) gets useless silica gel and soda ash in proportion, mix, be heated to 1250～1280 ℃ and make its fusing;
(2) the glass metal shrend after will melting, filter are done, oven dry, frit;
(3) with frit and other raw materials mix, carry out ball milling slurrying;
(4) the gained slurry is transferred to suitable concentration, adopts and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
(5) ceramic body after the glazing burns till under 1000 ℃, insulation 1h, and furnace cooling gets goods.
6. zirconium opaque enamel of raw material is characterized in that comprising following raw materials by weight percent:
Useless silica gel 32-56%
Silica sand 0-23%
Feldspar 16-41%
Wingdale 2-12%
Aluminum oxide 0-8.4%
Zinc oxide 0-4.3%
Fluorite 2.9-4.8%
Kaolin 0-17.5%
Natural manganese dioxide 0-1%.
7. zirconium opaque enamel of raw material according to claim 6 is characterized in that: said useless silica gel mainly is made up of silicon-dioxide and zirconium white, and wherein, zirconic content is the 5-12wt% of useless silica gel.
8. the preparation method of the described zirconium opaque enamel of raw material of claim 6 is characterized in that, may further comprise the steps:
(1), carries out ball milling slurrying with each raw materials mix;
(2) the gained slurry is transferred to suitable concentration, adopts and to soak glaze, be coated with glaze or glaze spraying is put into mode to the ceramic body glazing;
(3) with the body drying after the glazing, burn till at 1200-1280 ℃ then, insulation 0.5-1h, furnace cooling gets goods.
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| CN106145664A (en) * | 2016-06-28 | 2016-11-23 | 美轲（广州）化学股份有限公司 | Complex silicate zirconium opacifiers and preparation method and application |
| CN106630622A (en) * | 2016-12-29 | 2017-05-10 | 成都旭光电子股份有限公司 | Opaque glaze, and preparation method and application of opaque glaze |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104609901A (en) * | 2015-02-05 | 2015-05-13 | 洛阳师范学院 | Leadless and cadmiumless transparent glaze and preparation method thereof |
| CN104609901B (en) * | 2015-02-05 | 2016-08-24 | 洛阳师范学院 | A kind of lead-free and cadmium-free clear frit and preparation method thereof |
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| CN106145664B (en) * | 2016-06-28 | 2018-08-14 | 美轲（广州）化学股份有限公司 | Complex silicate zirconium opacifiers and the preparation method and application thereof |
| CN106630622A (en) * | 2016-12-29 | 2017-05-10 | 成都旭光电子股份有限公司 | Opaque glaze, and preparation method and application of opaque glaze |
| CN106630622B (en) * | 2016-12-29 | 2019-06-14 | 成都旭光电子股份有限公司 | A kind of opaque glaze and its preparation method and application |
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