CN105753325A - Decoration method for ceramic over-glaze pigment with high alkali resistance - Google Patents

Decoration method for ceramic over-glaze pigment with high alkali resistance Download PDF

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CN105753325A
CN105753325A CN201610044259.5A CN201610044259A CN105753325A CN 105753325 A CN105753325 A CN 105753325A CN 201610044259 A CN201610044259 A CN 201610044259A CN 105753325 A CN105753325 A CN 105753325A
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glaze
alkali resistance
color
ludox
quartz
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CN105753325B (en
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卢希龙
曹春娥
董俊方
冯涛
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Jingdezhen Ceramic Institute
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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
    • C03C8/02Frit compositions, i.e. in a powdered or comminuted form
    • 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
    • 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
    • C04B41/52Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/89Coating or impregnation for obtaining at least two superposed coatings having different compositions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a decoration method for ceramic over-glaze pigment with high alkali resistance.The ceramic over-glaze pigment comprises, by weight, 24% of quartz, 46.7% of boric acid, 11.7% of aluminum oxide, 3.7% of lithium carbonate, 1.6% of potassium nitrate, 1.2% of sodium carbonate, 6.5% of light calcium carbonate, 0.7% of niobium pentoxide and 3.9% of tantalum pentoxide.The decoration method includes supplementing deficient quartz materials in a silica sol form into molten fusing agents in a matched manner after the fusing agents are molten instead of adding the quartz materials into the fluxing agents when the fluxing agents are mixed with one another; carrying out enamel firing; coating the fusing agents and the quart materials with silica sol, sodium water glass and potassium water glass and then carrying out secondary enamel firing to obtain high-aluminum cover layers.The decoration method has the advantages that triple protection effects can be realized by the high-aluminum cover layers, the compounded and added silica sol instead of the quartz and transition metal oxide and the like, and accordingly the ceramic over-glaze colored pigment with the alkali resistance meeting 0-grade standards during European Union dishwasher safety tests can be obtained; the melting temperatures of the fusing agents can be reduced, accordingly, energy consumption can be reduced to a great extent, and the decoration method has an obvious economic benefit.

Description

A kind of trailing of high alkali resistance ceramic glazing dyestuff
Technical field
The invention belongs to ceramic glazing dyestuff technical field, be specifically related to the trailing of a kind of high alkali resistance ceramic glazing dyestuff.
Background technology
In recent years, day by day improve and the continuous of rhythm of life of people's living standard are accelerated, and are greatly promoted developing rapidly of the service trade such as food and drink, tourism, and increasing food and beverage enterprise even average family starts to select dish-washing machine that domestic ceramics tableware etc. is carried out.But alkaline auxiliary lotion, defoamer, oxidant, surfactant and the thickening agent etc. that contain in the cleaning mixture used by dish-washing machine, Conventional Portland goods had very strong corrosivity, especially tradition overglaze color ceramic there is stronger corrosiveness, overglaze color pottery after dish-washing machine cleans for a long time easily produces permanent surface damage, as faded, white opacity, iridescence, corrosion trace etc., have a strong impact on reusing of they, improve use cost.
Additionally, European Union is more and more harsher for the examination criteria of pottery machine washable, cause that China's overglaze color decorative daily-use tableware, hotel porcelain etc. are difficult to up to standard, thus cannot export sales smoothly, bring very big impact to China's domestic ceramics industry.Flux as pottery overglaze color important component part, for the corrosion proof impact of ornament materials on glaze it is critical that.
Ceramic decoration material refers to for materials such as all kinds of pigment of decorating ceramic articles, decal papers, wherein based on decorative pigment on glaze.But ceramic glazing dyestuff is mainly formulated by substantial amounts of flux and a certain amount of colorant, various pigment are added inking wet goods printing according to specific color theory simultaneously form by traditional decal paper.The performances such as the lead-indium alloy of ceramic decoration material, corrosion resistance are except the performance of colorant self, and it depends primarily on the content flux up to more than 70%, therefore at flux, the performances such as corrosion resistance is had significant impact.
The development of nano material is maked rapid progress, the application that constantly developing is new.Low melting point is one of principal character of nano material.Nano level Ludox and flux are mixed, the melt temperature of silicon oxide will be greatly reduced, just can form eutectic with flux at a lower temperature, at color roasting temperature, silicon oxide can dissolve in flux preferably, formed glass network structure, strengthen the acid resistance of flux, alkali resistance, wearability, microhardness, etc. performance indications.Additionally; some siliceous inorganic salt such as sodium silicate, potassium silicates etc.; can melt at a lower temperature; form high siliceous material; if these siliceous inorganic salts are coated on the flux of color roasting; carry out secondary color roasting; then these inorganic salts are easy to form eutectic with bottom flux; potassium, sodium etc. is infiltration downwards; the molecular level silicon oxide decomposed then is trapped in top layer, forms high silica glass one layer fine and close, as one layer of armor; flux is played a protective role, enhances the physical and chemical performance of flux.Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of technique is simple, environmental protection, alkali resistance is excellent, be suitable for the trailing of the high alkali resistance ceramic glazing dyestuff that dish-washing machine uses.
The present invention is achieved by the following technical programs: the trailing of a kind of high alkali resistance ceramic glazing dyestuff, it is characterised in that comprise the steps:
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, weighs other raw materials except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry acquisition flux standby;
Step 3: by step 2 gained flux and thin Ludox by weight percentage 35~38 62~65 mix after, by ceramic pigment on the 20 ~ 33% of flux weight additional glaze, obtain color painting on high alkali resistance ceramic glaze by evenly mixing afterwards;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: one or more in thick Ludox, sodium silicate, KP1 are mixed simultaneously, it is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, and furnace cooling obtains color painting decorative product on high alkali resistance ceramic glaze.
In described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm.
In described thick Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 20nm.
Ceramic pigment on ceramic pigment to be color roasting temperature the be glaze of 850 ~ 950 DEG C on described glaze.
The modulus of described sodium silicate is 1, and solid content is 60%.
The modulus of described KP1 is 1, and solid content is 50%.
Described thick Ludox, sodium silicate, KP1 mix in any proportion.
This patent adopts the method that mill adds Ludox, it is added without quartz raw material during flux dispensing, therefore, flux dispensing can be founded at a lower temperature, the quartz Ludox lacked coordinates supplementary in different proportions with flux, then color roasting, after making mixed liquor by Ludox, sodium silicate and KP1 etc., coating carries out secondary color roasting simultaneously, forms high silicon cap layer.On the one hand, compared with quartz bulky grain, it is nano level Ludox due to what add, SiO therein2Forming eutectic with flux at relatively low color roasting temperature, gained sample has higher glossiness;On the other hand, owing to having dissolved in equal even more SiO2So that glass network structure is finer and close, and the chemical stability of flux color roasting sample, physical property are all greatly improved;3rd, it is added without the quartz raw material of infusibility during owing to founding, is substantially reduced than the glass melting temperature of flux on traditional glaze.4th, the cap layer that secondary color roasting is formed is because of its SiO2Content is high, and its chemical stability is high, further increases the alkali resistance of sample.
The present invention adds with transition metal oxide compound by adopting Ludox to replace quartz and adopts the triple protections such as high silicon cap layer in sum; prepare the lead-free ceramics overglaze color pigment that alkali resistance is excellent, be suitable for dish-washing machine use; its alkali resistance reaches to meet 0 grade standard optimum shown in the resistance to machine testing standard that washes the dishes of European Union; reduce the glass melting temperature of flux simultaneously; significantly reduce energy consumption; therefore this pigment can be obviously improved China's domestic ceramics quality, has significant economic benefit.
Detailed description of the invention
For further setting forth that the present invention reaches technological means and effect that predetermined goal of the invention is taked, below in conjunction with preferred embodiment, the present invention is described in detail:
Embodiment 1
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 38g is mixed with thin Ludox 62g, ceramic pigment 7.9g on the dark blue glaze in additional sea, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.1g modulus, solid content be 60% sodium silicate be coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, and temperature retention time is 30min, and heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 104%, and alkali resistance grade is 0 grade.
Embodiment 2
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 38g is mixed with thin Ludox 62g, ceramic pigment 9.5g on the dark blue glaze in additional sea, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.04g modulus, solid content be 60% sodium silicate and 0.06g modulus be 1, solid content be 50% KP1 be coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, and furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, and after color roasting, sample is after testing, its glossiness is 103%, and alkali resistance grade is 0 grade.
Embodiment 3
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 38g is mixed with thin Ludox 62g, ceramic pigment 12.6g on the dark blue glaze in additional sea, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.03g modulus, solid content be 60% sodium silicate and 0.03g modulus be 1, solid content be 50% KP1 and 0.04g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 102%, and alkali resistance grade is 0 grade.
Embodiment 4
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 37g is mixed with thin Ludox 63g, ceramic pigment 7.4g on additional praseodymium zirconium yellow glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.05g modulus, solid content be 60% sodium silicate and 0.02g modulus be 1, solid content be 50% KP1 and 0.03g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 99%, and alkali resistance grade is 0 grade.
Embodiment 5
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 37g is mixed with thin Ludox 63g, ceramic pigment 9.3g on additional praseodymium zirconium yellow glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.1g modulus, solid content be 50% KP1 be coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, and temperature retention time is 30min, and heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 100%, and alkali resistance grade is 0 grade.
Embodiment 6
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 37g is mixed with thin Ludox 63g, ceramic pigment 12.3g on additional praseodymium zirconium yellow glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.03g modulus, solid content be 60% sodium silicate and 0.07g weight percentage be 30%, the thick Ludox that mean diameter is 0.02nm is coated uniformly on step 4 gained color roasting sample surfaces, puts into electric furnace after drying and carries out color roasting again, and color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, and furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, and after color roasting, sample is after testing, its glossiness is 101%, and alkali resistance grade is 0 grade.
Embodiment 7
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 36g is mixed with thin Ludox 64g, ceramic pigment 7.2g on additional chrome green glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.04g modulus, solid content be 60% sodium silicate and 0.04g modulus be 1, solid content be 50% KP1 and 0.02g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 100%, and alkali resistance grade is 0 grade.
Embodiment 8
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 36g is mixed with thin Ludox 64g, ceramic pigment 9.0g on additional chrome green glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.02g modulus, solid content be 50% KP1 and 0.08g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, puts into electric furnace after drying and carries out color roasting again, and color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, and furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, and after color roasting, sample is after testing, its glossiness is 99%, and alkali resistance grade is 0 grade.
Embodiment 9
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 36g is mixed with thin Ludox 64g, ceramic pigment 12.0g on additional chrome green glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.02g modulus, solid content be 60% sodium silicate and 0.05g modulus be 1, solid content be 50% KP1 and 0.03g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 101%, and alkali resistance grade is 0 grade.
Embodiment 10
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 35g is mixed with thin Ludox 65g, ceramic pigment 7.0g on additional gorgeous black glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.02g modulus, solid content be 60% sodium silicate and 0.06g modulus be 1, solid content be 50% KP1 and 0.02g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 102%, and alkali resistance grade is 0 grade.
Embodiment 11
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 35g is mixed with thin Ludox 65g, ceramic pigment 8.8g on additional gorgeous black glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 1 by 0.02g modulus, solid content be 60% sodium silicate and 0.02g modulus be 1, solid content be 50% KP1 and 0.06g weight percentage be 30%, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 99%, and alkali resistance grade is 0 grade.
Embodiment 12
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, by gross weight 100g other raw materials weighed except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry for standby;
Step 3: after step 2 gained flux 35g is mixed with thin Ludox 65g, ceramic pigment 11.6g on additional gorgeous black glaze, obtaining color painting on high alkali resistance ceramic glaze by evenly mixing afterwards, in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment 0.4g by 60 × 60mm area, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: be 30% by 0.1g weight percentage, the thick Ludox that mean diameter is 20nm is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, and temperature retention time is 30min, and heating rate is 5 DEG C/min, furnace cooling obtains color painting decoration sample on high alkali resistance ceramic glaze, after color roasting, sample is after testing, and its glossiness is 98%, and alkali resistance grade is 0 grade.
The test and evaluation method of glossiness and alkali resistance
By the glossiness of the WGG-60A type Grossmeters test color roasting sample that Shanghai Xin Rui instrument and meter company limited produces, with EU criteria BSEN12875-4:2006 " Mechanicaldishwashingresistanceofutensils-Part4:Rapidtes tfordomesticceramicarticles ", sample is carried out alkali resistance test, with the Assessment for classification method evaluation classification in EU criteria BSEN12875-2:2002 standard, its standard is as shown in the table:
European Union's Assessment for classification standard
Grade Cosmetic variation
0 Without visual change
1 Slight visual change
2 Substantially visual change

Claims (7)

1. the trailing of one kind high alkali resistance ceramic glazing dyestuff, it is characterised in that comprise the steps:
Step one: form by formula as below percentage by weight: quartz 24%, boric acid 46.7%, aluminium oxide 11.7%, lithium carbonate 3.7%, potassium nitrate 1.6%, sodium carbonate 1.2%, precipitated calcium carbonate 6.5%, niobium pentaoxide 0.7%, tantalum pentoxide 3.9%, weighs other raw materials except quartz;
Step 2: compound step one weighed grinds uniformly, after crossing 60 mesh sieves, load in corundum crucible, then corundum crucible is put in electric furnace and found, by the heating rate of 5 DEG C/min, it is warming up to 1150 DEG C, and after being incubated 60min, high-temperature fusant is poured rapidly quenching in cold water into, after wet ball grinding, cross 380 mesh sieves, dry acquisition flux standby;
Step 3: by step 2 gained flux and thin Ludox by weight percentage 35~38 62~65 mix after, by ceramic pigment on the 20 ~ 33% of flux weight additional glaze, obtain color painting on high alkali resistance ceramic glaze by evenly mixing afterwards;
Step 4: be coated uniformly on flat porcelain plate by step 3 gained pigment, put into electric furnace color roasting after drying, by the heating rate of 5 DEG C/min, is warming up to 900 DEG C, and is incubated 30min, furnace cooling;
Step 5: one or more in thick Ludox, sodium silicate, KP1 are mixed simultaneously, it is coated uniformly on step 4 gained color roasting sample surfaces, put into electric furnace after drying and carry out color roasting again, color roasting temperature is 920 DEG C, temperature retention time is 30min, heating rate is 5 DEG C/min, and furnace cooling obtains color painting decorative product on high alkali resistance ceramic glaze.
2. method according to claim 1, it is characterised in that: in described thin Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 6nm.
3. method according to claim 1, it is characterised in that: in described thick Ludox, the weight percentage of silicon oxide is 30%, and mean diameter is 20nm.
4. method according to claim 1, it is characterised in that: ceramic pigment on ceramic pigment to be color roasting temperature the be glaze of 850 ~ 950 DEG C on described glaze.
5. method according to claim 1, it is characterised in that: the modulus of described sodium silicate is 1, and solid content is 60%.
6. method according to claim 1, it is characterised in that: the modulus of described KP1 is 1, and solid content is 50%.
7. method according to claim 1, it is characterised in that: described thick Ludox, sodium silicate, KP1 mix in any proportion.
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CN107858018A (en) * 2017-10-17 2018-03-30 重庆工业职业技术学院 The special colouring pigment of ceramic sintering
CN110128854A (en) * 2019-05-28 2019-08-16 江苏拜富科技有限公司 Ceramic wine bottle low temperature pigment against corrosion acid and alkali-resistance flux
CN111072283A (en) * 2019-12-28 2020-04-28 福建省德化县溢茂工艺有限公司 Preparation process for preparing high-alkali-resistance ceramic glazing solvent by grinding and adding silica sol
CN112624614A (en) * 2020-12-25 2021-04-09 唐山北方瓷都陶瓷集团卫生陶瓷有限责任公司 High-wear-resistance ceramic glaze and preparation method thereof
CN113105267A (en) * 2021-04-13 2021-07-13 景德镇陶瓷大学 Ceramic stained paper additive, ceramic stained paper, selenium-rich ceramic and preparation method

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CN103044082A (en) * 2012-12-24 2013-04-17 醴陵市红玉红瓷陶瓷研究中心 Luminescent glaze for enamel painted porcelain and preparation method and application thereof
CN105198495A (en) * 2015-10-20 2015-12-30 佛山市华意陶瓷颜料有限公司 Small-particle-diameter praseodymium zirconium yellow ceramic pigment and preparation method thereof

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CN102234202A (en) * 2010-04-27 2011-11-09 重庆工商大学 Preparation method and glazing technology of ultra-low temperature red glaze additive
CN103044082A (en) * 2012-12-24 2013-04-17 醴陵市红玉红瓷陶瓷研究中心 Luminescent glaze for enamel painted porcelain and preparation method and application thereof
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Publication number Priority date Publication date Assignee Title
CN107858018A (en) * 2017-10-17 2018-03-30 重庆工业职业技术学院 The special colouring pigment of ceramic sintering
CN110128854A (en) * 2019-05-28 2019-08-16 江苏拜富科技有限公司 Ceramic wine bottle low temperature pigment against corrosion acid and alkali-resistance flux
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CN111072283A (en) * 2019-12-28 2020-04-28 福建省德化县溢茂工艺有限公司 Preparation process for preparing high-alkali-resistance ceramic glazing solvent by grinding and adding silica sol
CN112624614A (en) * 2020-12-25 2021-04-09 唐山北方瓷都陶瓷集团卫生陶瓷有限责任公司 High-wear-resistance ceramic glaze and preparation method thereof
CN113105267A (en) * 2021-04-13 2021-07-13 景德镇陶瓷大学 Ceramic stained paper additive, ceramic stained paper, selenium-rich ceramic and preparation method

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