CN101182236A - Zirconium silicate coated ceramic pigment and method for making same - Google Patents
Zirconium silicate coated ceramic pigment and method for making same Download PDFInfo
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- CN101182236A CN101182236A CNA2007100314009A CN200710031400A CN101182236A CN 101182236 A CN101182236 A CN 101182236A CN A2007100314009 A CNA2007100314009 A CN A2007100314009A CN 200710031400 A CN200710031400 A CN 200710031400A CN 101182236 A CN101182236 A CN 101182236A
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Abstract
The invention provides a zirconium silicate enwrapped ceramic pigment which comprises a color body and also comprises a shell body of metal oxide which is compounded by the zirconium silicate, and the shell body enwraps the color body compactly and completely. The invention also provides a preparation method of the zirconium silicate enwrapped ceramic pigment. Because accelerant is introduced into the preparation process, the method has the advantages that the loss of the color body is little; the enwrapping layer of the pigment is compact; the enwrapping rate is high; no thermal treatment of high temperature is required during the preparation process etc.
Description
Technical field
The present invention relates to a kind of ceramic pigment, particularly a kind of Zirconium silicate coated ceramic pigment and preparation method thereof
Background technology
Because the firing temperature higher (generally at 1000～1300 ℃) of ceramic, so the colorant that is applied to ceramic product not only color development ability is eager to excel, tone is pure, and in firing range, the thermostability of colorant will be got well, and can hold out against the erosion of glass melt.
The many mineral compound of occurring in nature have bright-coloured color and luster and colour generation ability, are referred to as the body that develops the color, as cadmium sulfoselenide (bright red), and Cadmium Sulfide (rheum officinale) and carbon black.Yet the high-temperature stability of these inorganic colors is relatively poor, is generally just being decomposed by complete oxidation more than 800 ℃.Thereby the application of these mineral compound has been subjected to very big restriction.
In order to improve the high-temperature stability of these mineral compound, widen the use temperature scope of colorant, some oxide compound or silicate mineralss that do not have color and have a high-temperature stability itself are used to wrap up these inorganic colors.Wherein, the mineral compound of colour developing is as the nuclear in these colorants, and has the oxide compound of high-temperature stable of reactionlessness or silicate minerals as shell, forms the coated colorant with nucleocapsid structure.Generally the Chang Yong method for preparing coated ceramic pigment is; body and integument precursor and mineralizer co-precipitation formation pre-reaction material will develop the color; again the sealing or under protective atmosphere high temperature burn till; this preparation method's defective is; the colour developing body easily distils in heat treatment process or is broken down and oxidized and causes a large amount of losses, encapsulation ratio to be difficult to that new breakthrough is arranged.Also there is data to propose, prepares the parcel precursor, make the integument densification with hydrothermal treatment consists again with common method, it is advantageous that subzero treatment, the colour developing body loses hardly, but this simple transformation becomes hydrothermal treatment process, it is extremely low to be difficult to successfully parcel or encapsulation ratio, can't reach industrialization level.The key that hydrothermal treatment consists prepares coated ceramic pigment is to make integument to reach densification easily, the parcel defective is few.Therefore, the present technique field needs a kind of new coated ceramic pigment preparation method, reaches the easy densification of integument in the hydrothermal treatment consists process, the few characteristics of parcel defective, makes that the ceramic pigment parcel for preparing is complete, fine and close.
Summary of the invention
Based on the deficiencies in the prior art, main purpose of the present invention is to provide a kind of Zirconium silicate coated ceramic pigment and preparation method thereof, subzero treatment on the technology, and the colour developing body loses hardly, colorant integument densification simultaneously, the parcel defective is few.
The present invention provides a kind of Zirconium silicate coated ceramic pigment in order to realize above-mentioned technical purpose, comprises the colour developing body and is wrapped in external housing of colour developing, and described housing is the mixture of zirconium silicate complex metal oxides.
Preferably, the colour developing body is cadmium sulfoselenide, Cadmium Sulfide, carbon black, sulphur, copper, ferric oxide, manganese oxide, chromic oxide, titanium oxide or Praseodymium trioxide.
Preferably, the metal oxide in the housing is a kind of or combination of the oxide compound of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium.More preferably, metal oxide is a kind of or combination of the oxide compound of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium.
Compared with prior art, in the housing of Zirconium silicate coated ceramic pigment provided by the invention, except zirconium silicate, also compound other metal oxides.The introducing of other metal oxides helps the production of zirconium silicate crystal under hydrothermal condition and the densification of zirconium silicate housing, and is fully fine and close to colour developing body parcel, the encapsulation ratio height.When the metal oxide in the housing was oxide compound a kind of of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium or combination, the parcel effect was finer and close than other metal oxides; Wherein, the oxide compound of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium is for better.
The present invention also provides a kind of method for preparing Zirconium silicate coated ceramic pigment, may further comprise the steps:
(1) preparation colour developing body;
(2) adopt co-precipitation/sol-gel method to coat zirconium silicate integument precursor at colour developing body surface layer;
(3) hydrothermal treatment consists makes zirconium silicate integument precursor conversion be fine and close integument;
(4) cooling, dry colorant;
In the solution of synthetic silicic acid zirconium integument precursor, introduce the accelerator solution of short integument densification, described accelerator solution comprises the metal soluble salt, and the pH value of maintenance mixed solution system is between 6～12.
Preferably, comprise one or more combinations of the soluble salt of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium in the accelerator solution.More preferably, comprise one or more combinations of the soluble salt of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium in the accelerator solution.
The ratio of the mole number sum of the zirconates of the mole number sum of solubility salt and synthetic silicic acid zirconium integument precursor, silicon compound is 0.0001～0.3 in the described accelerator solution.
In the hydrothermal treatment consists process, temperature of reaction is 200～500 ℃, and reaction pressure is 0.2～110MPa, and the reaction times is 1～24 hour.The content of mineralizer is 0.1～10% in the zirconium silicate integument precursor.
Compared with prior art, the preparation method of Zirconium silicate coated ceramic pigment of the present invention introduces the accelerator solution of urging the integument densification, and promotor comprises the metal soluble salt.When utilizing collosol and gel/coprecipitation method to coat the zirconium silicate presoma in the colour developing surface, the substance change that from accelerator solution, generates the surface energy of colour developing body, improved the chemical affinity of colour developing body and coating layer, help the coating of zirconium silicate presoma to the body that develops the color; And in the hydrothermal treatment consists process, the material that generates from accelerator solution can generate transition phase with silicon oxide and zirconium white in the zirconium silicate forming process, reduce the crystallization activation energy of zirconium silicate, accelerate the crystallization speed of zirconium silicate, help the zirconium silicate densification of crystallization and zirconium silicate shell in the short period of time.Therefore the colorant for preparing, it is little to have a colour developing bulk diffusion, the densification of colorant integument, the encapsulation ratio advantages of higher, and also preparation process need pass through high-temperature heat treatment, the minimizing energy consumption.
For making the present invention easier to understand, below further set forth the specific embodiment of Zirconium silicate coated ceramic pigment of the present invention and preparation method thereof.
Embodiment
In a Zirconium silicate coated ceramic pigment preparation method's of the present invention specific embodiment, may further comprise the steps:
(1) preparation of colour developing body;
With 0.001 mole of CdCl
2Fully be dissolved in the 100mL distilled water and obtain solution A; Na with 0.001 mole
2S fully is dissolved in the 100mL distilled water and obtains solution B.After in 100mL water, adding stablizer and tensio-active agent, A and B are slowly splashed under stirring condition, and feed nitrogen simultaneously.Treat A liquid and B drop add finish after, add coupling agent, continue to stir certain hour, make Cadmium Sulfide.
(2) adopt co-precipitation/sol-gel method to coat zirconium silicate integument precursor at colour developing body surface layer;
The Cadmium Sulfide suspended dispersed for preparing in distilled water, is transferred to 6 with the pH value of suspension, splash into the solution that 20mL concentration is 0.0001mol/L zirconium oxychloride, water glass and tin protochloride respectively.With being dispersed in after the throw out centrifugation in the mixing solutions of 100mL ethanol and ammoniacal liquor (ammonia concn 4.2vol%), subsequently, under stirring condition, splash into the 5mL tetraethoxy.After continuing to stir 1h, the product centrifugation separation, the cryodrying that obtain.
(3) hydrothermal treatment consists makes zirconium silicate integument precursor conversion be fine and close integument;
Throw out is transferred in the hydrothermal reaction kettle, add 10%NaF and NaOH after, be 80% at 240 ℃, filling ratio, carry out hydro-thermal reaction under 7 hours the condition of insulation, make xanchromatic zirconium silicate parcel Cadmium Sulfide high temperature decorating colour.
(4) cooling, dry colorant.
The zirconium silicate that obtains parcel cadmium sulfide ceramic colorant has comprised Cadmium Sulfide and has been wrapped in the housing of Cadmium Sulfide outside that housing is the compound of zirconium silicate composite tin oxide, and housing is fine and close to the Cadmium Sulfide parcel, fully.
In another specific embodiment of Zirconium silicate coated ceramic pigment preparation method of the present invention, may further comprise the steps:
(1) preparation of colour developing body;
With 0.005 mole of CdCl
2Fully be dissolved in the 100mL distilled water and obtain solution C; With a certain proportion of Na
2S, selenium powder and NaOH fully are dissolved in the 100mL distilled water and obtain solution D.After in 100mL water, adding stablizer and tensio-active agent, C and D are slowly splashed under stirring condition.Treat C liquid and D drop add finish after, add coupling agent, continue to stir certain hour, make cadmium sulfoselenide.
(2) adopt co-precipitation/sol-gel method to coat zirconium silicate integument precursor at colour developing body surface layer;
The cadmium sulfoselenide suspended dispersed for preparing in distilled water, is transferred to 12 with the pH value of suspension, splash into the solution that 20mL concentration is 0.0003mol/L zirconium oxychloride, water glass and tantalum chloride respectively.With being dispersed in after the throw out centrifugation in the mixing solutions of 100mL ethanol and ammoniacal liquor (ammonia concn 4.2vol%), subsequently, under stirring condition, splash into the 7mL tetraethoxy.After continuing to stir 1h, the product centrifugation separation, the cryodrying that obtain.
(3) hydrothermal treatment consists makes zirconium silicate integument precursor conversion be fine and close integument;
Throw out is transferred in the hydrothermal reaction kettle, add 10%KF and KOH after, be 75% at 300 ℃, filling ratio, carry out hydro-thermal reaction under 5 hours the condition of insulation, make red zirconium silicate parcel cadmium sulfoselenide high temperature decorating colour.
(4) cooling, dry colorant.
The zirconium silicate that obtains parcel cadmium sulfoselenide ceramic pigment has comprised cadmium sulfoselenide and has been wrapped in the housing of cadmium sulfoselenide outside that housing is the compound of zirconium silicate combined oxidation tantalum, and housing is fine and close to the cadmium sulfoselenide parcel, fully.
In another specific embodiment of Zirconium silicate coated ceramic pigment preparation method of the present invention, may further comprise the steps:
(1) preparation of colour developing body;
0.01g carbon dust, 0.002mol cetyl trimethylammonium bromide are joined in the 100mL distilled water, and ultra-sonic dispersion obtained suspension E in 10 minutes.
(2) adopt co-precipitation/sol-gel method to coat zirconium silicate integument precursor at colour developing body surface layer;
After with the sodium hydroxide solution of 0.1mol/L the pH value of E being transferred to 9.5, splash into the solution that 20mL concentration is 0.0003mol/L zirconium oxychloride, water glass, calcium chloride and aluminum chloride respectively.With being dispersed in after the throw out centrifugation in the mixing solutions of 100mL ethanol and ammoniacal liquor (ammonia concn 4.2vol%), subsequently, under stirring condition, splash into the 7mL tetraethoxy.After continuing to stir 1h, the product centrifugation separation, the cryodrying that obtain.
(3) hydrothermal treatment consists makes zirconium silicate integument precursor conversion be fine and close integument;
Throw out is transferred in the hydrothermal reaction kettle, add 10%KCl and NaF after, be 70% at 350 ℃, filling ratio, carry out hydro-thermal reaction under 3 hours the condition of insulation, make the zirconium silicate parcel carbon dust high temperature decorating colour of black.
(4) cooling, dry colorant.
The zirconium silicate that obtains parcel carbon dust ceramic pigment has comprised carbon dust and has been wrapped in the housing of carbon dust outside that housing is the hopcalite of the compound calcium of zirconium silicate, aluminium, and housing is fine and close to the carbon dust parcel, fully.
In Zirconium silicate coated ceramic pigment preparation method's of the present invention embodiment, can comprise one or more combinations of the soluble salt of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium in the accelerator solution, be preferably one or more combinations of the soluble salt of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium.The colour developing body can also be sulphur, copper, ferric oxide, manganese oxide, chromic oxide, titanium oxide or Praseodymium trioxide.The ratio of the mole number sum of the zirconates of the mole number sum of solubility salt and synthetic silicic acid zirconium integument precursor, silicon compound can be 0.0001～0.3 in the accelerator solution.In the hydrothermal treatment consists process, temperature of reaction is 200～500 ℃, and reaction pressure is 0.2～110MPa, and the reaction times is 1～24 hour.The content of mineralizer is 0.1～10% in the zirconium silicate integument precursor.
Compared with prior art, the colorant that adopts the preparation method of Zirconium silicate coated ceramic pigment of the present invention to obtain, it is little to have a colour developing bulk diffusion, the densification of colorant integument, the encapsulation ratio height, preparation process need be through advantages such as high-temperature heat treatment.
Above disclosed only is the preferred embodiment of Zirconium silicate coated ceramic pigment of the present invention and preparation method thereof, certainly can not limit the present invention's interest field with this, therefore the equivalent variations of being done according to the present patent application claim still belongs to the scope that the present invention is contained.
Claims (10)
1. Zirconium silicate coated ceramic pigment comprises the colour developing body and is wrapped in the housing of external of colour developing, it is characterized in that described housing is the mixture of zirconium silicate complex metal oxides.
2. Zirconium silicate coated ceramic pigment as claimed in claim 1 is characterized in that, the metal oxide in the described housing is a kind of or combination of the oxide compound of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium.
3. Zirconium silicate coated ceramic pigment as claimed in claim 1 is characterized in that, the metal oxide in the described housing is a kind of or combination of the oxide compound of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium.
4. Zirconium silicate coated ceramic pigment as claimed in claim 1 is characterized in that, described colour developing body is cadmium sulfoselenide, Cadmium Sulfide, carbon black, sulphur, copper, ferric oxide, manganese oxide, chromic oxide, titanium oxide or Praseodymium trioxide.
5. method for preparing Zirconium silicate coated ceramic pigment as claimed in claim 1 may further comprise the steps:
(1) preparation colour developing body;
(2) adopt co-precipitation/sol-gel method to coat zirconium silicate integument precursor at colour developing body surface layer;
(3) hydrothermal treatment consists makes zirconium silicate integument precursor conversion be fine and close integument;
(4) cooling, dry colorant;
It is characterized in that in the solution of synthetic silicic acid zirconium integument precursor, introduce the accelerator solution of short integument densification, described accelerator solution comprises the metal soluble salt, and the pH value of maintenance mixed solution system is between 6～12.
6. the preparation method of Zirconium silicate coated ceramic pigment as claimed in claim 5 is characterized in that, comprises one or more combinations of the soluble salt of alkaline-earth metal, rare earth metal, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium in the described accelerator solution.
7. the preparation method of Zirconium silicate coated ceramic pigment as claimed in claim 6, it is characterized in that, comprise one or more combinations of the soluble salt of calcium, magnesium, scandium, yttrium, lanthanum, cerium, praseodymium, rubidium, tin, tantalum, manganese, vanadium, titanium, molybdenum or aluminium in the described accelerator solution.
8. the preparation method of Zirconium silicate coated ceramic pigment as claimed in claim 5, it is characterized in that the ratio of the mole number sum of the zirconates of the mole number sum of solubility salt and synthetic silicic acid zirconium integument precursor, silicon compound is 0.0001～0.3 in the described accelerator solution.
9. the preparation method of Zirconium silicate coated ceramic pigment as claimed in claim 5 is characterized in that, in the described hydrothermal treatment consists process, temperature of reaction is 200～500 ℃, and reaction pressure is 0.2～110MPa, and the reaction times is 1～24 hour.
10. the preparation method of Zirconium silicate coated ceramic pigment as claimed in claim 5 is characterized in that, the content of mineralizer is 0.1～10% in the described zirconium silicate integument precursor.
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| CN101786902A (en) * | 2010-03-04 | 2010-07-28 | 陕西科技大学 | Preparation method for extended red ZrSiO_4-Cd (S_xSe_(1-x)) pigment |
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