CN101353487A - Multi-layer multi-color changing colour change interval pigment and preparation thereof - Google Patents
Multi-layer multi-color changing colour change interval pigment and preparation thereof Download PDFInfo
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Abstract
The invention provides a multi-layer multi-color transition interval pigment and a preparation method thereof, relating to the field of pigment. Mica film or glass film is used as the substrate; multiple metal oxide layers are covered alternately on the surface of the substrate; the first, third and fifth layers are high-refractive index metal oxide with the refractive index higher than 2.0; the second and forth layers are low-refractive index oxide with the refractive index lower than 1.8. The pigment has bright color and obvious color changing; the preparation method utilizes wet chemical hydrolysis process to alternately cover multiple oxide layers on the surface of the substrate. The method has reasonable structure, advanced process, easy operation, stable product quality and suitability to industrialized production.
Description
Technical field
The present invention relates to pigment and preparation field thereof, relate in particular to multi-layer multi-color changing colour change interval pigment and preparation method thereof.
Background technology
Along with the development of pigment, people have developed high-performance effect pigment-camouflage paint of new generation.
So-called multiple-layer alteration paint can present the continuous variation of the color between two or more interference color with the viewing angle difference.
Oxide-coated reaches certain thickness with coating on flat substrates, when light is mapped to coatingsurface, a part is injected light wave and is reflected, part light is transmitted to down layer of surface by coating, produces reflection of light and transmission again, will produce " interference " phenomenon of light like this.If following n represents the coating refractive index, d is a coat-thickness, and then nd is the optical thickness of coating.Some catoptrical reflected light wavelength λ=2nd/N, N is a positive integer, is weakened by interference effect, other reflected light (λ=4nd/ (2N-1)) are enhanced.
When the oxide compound of high refractive index and the oxide compound of low refractive index alternately are coated on the flat substrates, when wherein two-layer or multilayer had identical optical thickness, so catoptrical color can increase along with the increase of the number of plies.But also can be by suitable design and the thickness of selecting coat, also can be strong especially as the color change of visual angle function.The basis that Here it is prepares strong interference pigment and effect interference pigment.
Present multiple-layer alteration paint is to pass through the multilayered structure that vapor phase process or wet chemical method coated metal oxide and nonmetal oxide form on the surface of substrate.Because the difference of substrate, the production method of its pigment is also inequality.Multiple-layer alteration paint is broadly divided into transparent (approximate transparent) and opaque (sub-opaque) two big classes, transparent (approximate transparent) is as the Color Stream pigment of German Merck company, be to be base material, and then carry out with wet chemical method that titanium dioxide or ferric oxide deposition coating make with the silicon-dioxide thin slice.The Varocrom pigment as German BASF AG of opaque (sub-opaque) is to be base material with metal aluminium flake or oxidation iron plate, coated silica again, and this process is finished in fluidized-bed reactor.
In recent years, it is base material that multinomial patent has proposed with nonmetal or metallic compound, adopted liquid-phase chemistry deposition technique, rely on high and low refractive index material alternate multiple cladding process to prepare the method for camouflage paint, because of every technology difference, the transition interval of camouflage paint is also different, mainly is two or three transition intervals.
The creativity and innovation content
One of purpose of the present invention provides a kind of multi-layer multi-color changing colour change interval pigment.
Two of purpose of the present invention provides a kind of preparation method of multi-layer multi-color changing colour change pigment.
For achieving the above object, a kind of multi-layer multi-color changing colour change interval pigment of the present invention comprises one deck substrate, alternately coats multilevel oxide on the surface of substrate, and transition interval is along with the increase of the number of plies increases synchronously.First and third, five layers of odd-level is specific refractory power greater than 2.0 metal oxide; The second, four layers of even level is specific refractory power less than 1.8 metal oxide.
Above-mentioned substrate comprises natural mica thin slice or synthetic mica sheet or glass flake, and its thickness is 0.2-3um, and particle diameter is the thin slice of 10-300um, is approximately the planar structure.
First and third, five layer of above-mentioned odd-level is specific refractory power greater than 2.0 metal oxide is SnO
2Or TiO
2Or Fe
2O
3Or their mixture or mixture, every layer of clad ratio is respectively 10%-15%.
Second, four layer of above-mentioned even level is specific refractory power less than 1.8 metal oxide is SiO
2Or Al
2O
3Or B
2O
3Or their mixture or mixture, every layer of clad ratio is respectively 15%-20%.
The present invention also provides a kind of preparation method of above-mentioned multi-layer multi-color changing colour change interval pigment, and this method in turn includes the following steps:
(1) is that 10-300um, thickness are natural mica thin slice or synthetic mica sheet or the glass flake of 0.2-3um with particle diameter, presses 5%-10% (weight ratio) and drop in the deionized water that dispersed with stirring becomes to disperse suspension and is warmed up to 70 ℃-80 ℃.
(2) pH value with step (1) suspension transfers to 1.5-3.5 (when transferring pH value, with weight ratio 10% dilute hydrochloric acid or 15% sodium hydroxide solution, below respectively go on foot identical), be metered into the inorganic salt of specific refractory power greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, to keep PH constant by adding certain density sodium hydroxide simultaneously, behind reinforced finishing, constant temperature stirred 10-30 minute, form first coating layer this moment, and the specific refractory power in the solution enters first coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 corresponding oxide compound dissociates out.
(3) pH value of step (2) suspension is transferred 4-8, be metered into the inorganic salt of specific refractory power again less than 1.8 oxide compound correspondence, the clad ratio that makes oxide compound is 15%-20%, adding certain density sodium hydroxide or dilute hydrochloric acid simultaneously, to keep pH value constant, constant temperature stirred 10-30 minute behind reinforced finishing, form second coating layer this moment, and specific refractory power enters second coating layer less than the oxide compound that the soluble inorganic salt of 1.8 corresponding oxide compound dissociates out in the solution.
(4) PH with step (3) suspension transfers to 1.5-3.5, be metered into the inorganic salt of specific refractory power again greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, adding certain density sodium hydroxide simultaneously, to keep pH value constant, behind reinforced finishing, constant temperature stirred 10-30 minute, and form the 3rd coating layer this moment, and specific refractory power enters the 3rd coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 oxide compound correspondence dissociates out in the solution.
(5) the suspension PH with step (4) transfers to 4-8, be metered into the inorganic salt of specific refractory power again less than 1.8 oxide compound correspondence, the clad ratio that makes oxide compound is 15%-20%, adding certain density sodium hydroxide or dilute hydrochloric acid simultaneously, to keep pH value constant, constant temperature stirred 10-30 minute behind reinforced finishing, form the 4th coating layer this moment, and specific refractory power enters the 4th coating layer less than the oxide compound that the soluble inorganic salt of 1.8 corresponding oxide compound dissociates out in the solution.
(6) PH with step (5) suspension transfers to 1.5-3.5, be metered into the inorganic salt of specific refractory power again greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, adding certain density sodium hydroxide simultaneously, to keep pH value constant, behind reinforced finishing, constant temperature stirred 10-30 minute, and form the 5th coating layer this moment, and specific refractory power enters the 5th coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 oxide compound correspondence dissociates out in the solution.
(7) with the suspension filtered of step (6), use the deionized water wash filtrate, 100 ℃ of-150 ℃ of oven dry, the 60-100 mesh sieve is crossed in 500 ℃-750 ℃ calcinings after 20-30 minute, get product.
Above-mentioned specific refractory power is a chlorate greater than the solubility inorganic metal salt of 2.0 oxide compound correspondence, as SnCl
4Or TiCl
4Or FeCl
3
Above-mentioned specific refractory power less than the soluble inorganic salt of 1.8 oxide compound correspondence is: Na
2SiO
3Or AlCl
3Or Na
2B
4O
7
Above-mentioned preparation method adopts the wet-chemical hydrolysis process, the pH value fluctuation range in the reactor is controlled at ± 0.05 in, strict guarantee the quality that coats of multilayer.
This multi-layer multi-color changing colour change interval pigment is mainly used in industries such as coating, printing ink, makeup, leather, plastic and glass.
The present invention has following beneficial effect:
Multi-layer multi-color changing colour change interval pigment transition interval of the present invention is five, changes continuously by green-indigo plant-purple-red-xanchromatic from vertically watching to the horizontal view angle promptly, and bright in luster, color changeable effect is obvious.
The preparation method of multi-layer multi-color changing colour change interval pigment of the present invention is rational in infrastructure, technology advanced person, and easy handling, constant product quality.
Specific embodiment
The following examples are used for explaining in more detail the present invention, but do not limit the present invention.
Embodiment 1:
The structure of pigment is: Fe
2O
3| SiO
2| Fe
2O
3| SiO
2| Fe
2O
3| sheet glass
The deionized water that adds 1000 milliliters in 2.5 liters little reactor drops into particle diameter for 60-300um thickness is the sheet glass 100g of 0.6-3um, stirs into suspension and constant temperature to 75 ℃.
1. the pH value with above-mentioned suspension transfers to 3.5 (when transferring pH value, with weight ratio is 10% dilute hydrochloric acid or 15% sodium hydroxide solution, following steps are identical), metering drips ferric chloride aqueous solutions 423ml (concentration is 120g/L), to keep pH value constant by adding 15% sodium hydroxide solution simultaneously, behind reinforced finishing, constant temperature stirs and (forms first coating layer, the FeCl in the solution this moment in 15 minutes
3The Fe that disassociation is come out
2O
3Enter first coating layer).
2. transferring pH value is 8.0, and (concentration is for containing SiO for the sodium silicate solution that the metering dropping is 2.1 liters
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, (formed second coating layer, the SiO that the water glass in the solution dissociates out at this moment in 15 minutes when the reinforced back constant temperature that finishes stirs
2Enter second coating layer).
3. transferring pH value is 3.5, metering drips ferric chloride aqueous solutions 419ml (concentration is 120g/L), and to keep pH value constant by adding 15% sodium hydroxide solution simultaneously, behind reinforced finishing, constant temperature stirs and (forms the 3rd coating layer, the FeCl in the solution this moment in 15 minutes
3The Fe that disassociation is come out
2O
3Enter the 3rd coating layer;
4. transferring pH value is 8.0, and metering drips sodium silicate solution, and 1.92 liters (concentration is for containing SiO
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, (formed the 4th coating layer, the SiO that the water glass in the solution dissociates out at this moment in 15 minutes when the reinforced back constant temperature that finishes stirs
2Enter the 4th coating layer).
5. transferring pH value is 3.5, and metering drips 420 milliliters of liquor ferri trichloridis (concentration 120g/L).To keep pH value stable by dripping 15% sodium hydroxide solution simultaneously, (formed the 5th coating layer, the FeCl in the solution at this moment in 15 minutes when the reinforced back constant temperature that finishes stirs
3The Fe that disassociation is come out
2O
3Enter the 5th coating layer).
6, with suspension filtered, use deionized water wash, 120 ℃ of oven dry down, calcined 20 minutes for 500 ℃, cross 60 mesh sieves then, get product.(total clad ratio is 60%)
Through the card-coating test,, can see that its color is changed continuously by green-indigo plant-purple-red-yellow multicoloured interval from vertically watching to the horizontal view angle.
Embodiment 2
The structure of pigment is: Fe
2O
3| SiO
2+ B
2O
3| Fe
2O
3| SiO
2+ B
2O
3| Fe
2O
3| the synthetic mica thin slice
The deionized water that adds 1000 milliliters in 2.5 liters little reactor, the input particle diameter is that 30-150um, thickness are the synthetic mica thin slice 75g of 0.3-1.5um, stirs into suspension and constant temperature to 75 ℃.
1. the pH value with above-mentioned suspension transfers to 3.5 (when transferring pH value, with weight ratio 10% dilute hydrochloric acid or 15% sodium hydroxide solution, below identical), metering drips ferric chloride aqueous solutions 578ml (concentration is 120g/L), and to keep pH value constant by adding 15% sodium hydroxide solution simultaneously, behind reinforced finishing, constant temperature stirs and (forms first coating layer, the FeCl in the solution this moment in 15 minutes
3The Fe that disassociation is come out
2O
3Enter first coating layer).
2. pH value is transferred to 7.5, metering drips dobell's solution 44ml (concentration is 100g/L), and to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, behind reinforced finishing, and restir 15 minutes; Transferring pH value is 8.0, and metering drips sodium silicate solution, and 2.65 liters (concentration is for containing SiO
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, and behind reinforced finishing, restir (forms second coating layer, the B that Sodium Tetraborate in the solution and water glass dissociate out this moment in 15 minutes
2O
3And SiO
2Enter second coating layer).
3. transferring pH value is 3.5, metering drips ferric chloride aqueous solutions 565ml (concentration is 120g/L), and to keep pH value constant by adding 15% sodium hydroxide solution simultaneously, behind reinforced finishing, constant temperature stirs and (forms the 3rd coating layer, the FeCl in the solution this moment in 15 minutes
3The Fe that disassociation is come out
2O
3Enter the 3rd coating layer).
4. pH value is transferred to 7.5, metering drips dobell's solution 40ml (concentration is 100g/L), and to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, behind reinforced finishing, and restir 15 minutes; Transferring pH value is 8.0, and metering drips sodium silicate solution, and 2.5 liters (concentration is for containing SiO
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, and behind reinforced finishing, restir (forms the 4th coating layer, the B that Sodium Tetraborate in the solution and water glass dissociate out this moment in 15 minutes
2O
3And SiO
2Enter the 4th coating layer).
5. transferring pH value is 3.5, metering drips ferric chloride aqueous solutions 555ml (concentration is 120g/L), and to keep pH value constant by adding 15% sodium hydroxide solution simultaneously, behind reinforced finishing, constant temperature stirs and (forms the 5th coating layer, the FeCl in the solution this moment in 15 minutes
3The Fe that disassociation is come out
2O
3Enter the 5th coating layer).
6. with suspension filtered, use deionized water wash,, calcined 20 minutes for 550 ℃, cross 80 mesh sieves then, get product 120 ℃ of oven dry down.(total clad ratio is 72.5%)
Through the card-coating test,, can see that its color is changed continuously by green-indigo plant-purple-multicoloured interval of red-xanchromatic from vertically watching to the horizontal view angle.
Embodiment 3
The structure of pigment is: | TiO
2+ SnO
2| SiO
2+ Al
2O
3| TiO
2+ SnO
2| SiO
2+ Al
2O
3| TiO
2+ SnO
2| natural mica
The deionized water that adds 1000 milliliters in 2.5 liters little reactor, dropping into particle diameter again is that 10-60um, thickness are the natural mica 50g of 0.2-0.6um, stirs into suspension and constant temperature to 75 ℃.
1. the pH value with above-mentioned suspension transfers to 1.5 (when transferring pH value, with weight ratio 10% dilute hydrochloric acid or 15% sodium hydroxide solution, below identical), metering drips tin tetrachloride solution 30ml (concentration is 100g/L), dripping 15% sodium hydroxide solution simultaneously, to keep pH value constant, behind reinforced finishing, constant temperature stirred 15 minutes, transferring pH value is 2.1, metering drips titanium tetrachloride solution 1032ml (concentration 115g/L), and to keep pH value constant by dripping 15% sodium hydroxide solution simultaneously, when the reinforced back constant temperature stirring 15 minutes that finishes, (form first coating layer, the SnCl in the solution this moment
4And TiCl
4The SnO that disassociation is come out
2And TiO
2Enter first coating layer).
2. pH value is transferred to 4.0, metering drips AlCl
3Solution 88ml (concentration 100g/L), dripping 15% sodium hydroxide solution simultaneously, to keep pH value constant, and behind reinforced finishing, constant temperature stirred 15 minutes; Transferring pH value is 8.0, and metering drips sodium silicate solution, and 3.7 liters (concentration is for containing SiO
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, and behind reinforced finishing, restir (forms second coating layer, the Al that aluminum chloride in the solution and water glass dissociate out this moment in 15 minutes
2O
3And SiO
2Enter second coating layer).
3. transferring pH value is 1.5, metering drips tin tetrachloride solution 28ml (concentration is 100g/L), to keep pH value constant by dripping 15% sodium hydroxide solution simultaneously, and behind reinforced finishing, constant temperature stirred 15 minutes, transferring pH value is 2.1, metering drips titanium tetrachloride solution 1020ml (concentration 115g/L), and to keep pH value constant by dripping 15% sodium hydroxide solution simultaneously, when the reinforced back constant temperature stirring 15 minutes that finishes, (form the 3rd coating layer, the SnCl in the solution this moment
4And TiCl
4The SnO that disassociation is come out
2And TiO
2Enter the 3rd coating layer).
4. pH value is transferred to 4.0, metering drips AlCl
3Solution 84ml (concentration 100g/L), dripping 15% sodium hydroxide solution simultaneously, to keep pH value constant, and behind reinforced finishing, constant temperature stirred 15 minutes; Transferring pH value is 8.0, and metering drips sodium silicate solution, and 3.5 liters (concentration is for containing SiO
218g/L), to keep pH value constant by dripping 10% dilute hydrochloric acid solution simultaneously, and behind reinforced finishing, restir (forms the 4th coating layer, the Al that aluminum chloride in the solution and water glass dissociate out this moment in 15 minutes
2O
3And SiO
2Enter the 4th coating layer).
5. transferring pH value is 1.5, metering drips tin tetrachloride solution 26ml (concentration is 100g/L), to keep pH value constant by dripping 15% sodium hydroxide solution simultaneously, and behind reinforced finishing, constant temperature stirred 15 minutes, transferring pH value is 2.1, metering drips titanium tetrachloride solution 980ml (concentration 100g/L), and to keep pH value constant by dripping 15% sodium hydroxide solution simultaneously, when the reinforced back constant temperature stirring 15 minutes that finishes, (form the 5th coating layer, the SnCl in the solution this moment
4And TiCl
4The SnO that disassociation is come out
2And TiO
2Enter the 5th coating layer).
6. with suspension filtered, use deionized water wash,, calcined 20 minutes for 750 ℃, cross 100 mesh sieves then, get product 120 ℃ of oven dry down.(total clad ratio is 85%)
Through the card-coating test,, can see that its color is changed continuously by green-indigo plant-purple-multicoloured interval of red-xanchromatic from vertically watching to the horizontal view angle.
Claims (6)
1. multi-layer multi-color changing colour change interval pigment, it is characterized in that: described pigment comprises substrate, alternately coats the different oxide compound of multilayer on the surface of substrate, at odd-level, promptly first and third, five layer is specific refractory power greater than 2.0 metal oxide; At even level, promptly second, four layer is specific refractory power less than 1.8 oxide compound.
2. multi-layer multi-color changing colour change interval pigment as claimed in claim 1 is characterized in that described substrate is natural mica thin slice or synthetic mica sheet or glass flake, and its thickness is that 0.2-3um, particle diameter are the thin slice of 10-300um.
3. multi-layer multi-color changing colour change interval pigment as claimed in claim 1 or 2 is characterized in that first and third, five layer of odd-level specific refractory power is SnO greater than 2.0 metal oxide
2Or TiO
2Or Fe
2O
3Or their mixture or mixture, every layer of clad ratio is respectively 10%-15%; The second, four layers of even level specific refractory power is SiO less than 1.8 metal oxide
2Or Al
2O
3Or B
2O
3Or their mixture or mixture, every layer of clad ratio is respectively 15%-20%.
4. the preparation method of multi-layer multi-color changing colour change interval pigment as claimed in claim 3 in turn includes the following steps:
(1) thin slice is pressed 5%-10% (weight ratio) and dropped in the deionized water, dispersed with stirring becomes to disperse suspension and is warmed up to 70 ℃-80 ℃;
(2) pH value with step (1) suspension transfers to 1.5-3.5, when transferring pH value, with weight ratio 10% dilute hydrochloric acid or 15% sodium hydroxide solution, below respectively go on foot identical, be metered into the inorganic salt of specific refractory power greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, to keep PH constant by adding certain density sodium hydroxide simultaneously, behind reinforced finishing, constant temperature stirred 10-30 minute, form first coating layer this moment, and the specific refractory power in the solution enters first coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 corresponding oxide compound dissociates out;
(3) pH value of step (2) suspension is transferred 4-8, be metered into the inorganic salt of specific refractory power again less than 1.8 oxide compound correspondence, the clad ratio that makes oxide compound is 15%-20%, adding certain density sodium hydroxide or dilute hydrochloric acid simultaneously, to keep pH value constant, constant temperature stirred 10-30 minute behind reinforced finishing, form second coating layer this moment, and specific refractory power enters second coating layer less than the oxide compound that the soluble inorganic salt of 1.8 corresponding oxide compound dissociates out in the solution;
(4) PH with step (3) suspension transfers to 1.5-3.5, be metered into the inorganic salt of specific refractory power again greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, adding certain density sodium hydroxide simultaneously, to keep pH value constant, behind reinforced finishing, constant temperature stirred 10-30 minute, and form the 3rd coating layer this moment, and specific refractory power enters the 3rd coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 oxide compound correspondence dissociates out in the solution;
(5) the suspension PH with step (4) transfers to 4-8, be metered into the inorganic salt of specific refractory power again less than 1.8 oxide compound correspondence, the clad ratio that makes oxide compound is 15%-20%, adding certain density sodium hydroxide or dilute hydrochloric acid simultaneously, to keep pH value constant, constant temperature stirred 10-30 minute behind reinforced finishing, form the 4th coating layer this moment, and specific refractory power enters the 4th coating layer less than the oxide compound that the soluble inorganic salt of 1.8 corresponding oxide compound dissociates out in the solution;
(6) PH with step (5) suspension transfers to 1.5-3.5, be metered into the inorganic salt of specific refractory power again greater than 2.0 oxide compound correspondence, the clad ratio that makes oxide compound is 10%-15%, adding certain density sodium hydroxide simultaneously, to keep pH value constant, behind reinforced finishing, constant temperature stirred 10-30 minute, and form the 5th coating layer this moment, and specific refractory power enters the 5th coating layer greater than the oxide compound that the soluble inorganic salt of 2.0 oxide compound correspondence dissociates out in the solution;
(7) with the suspension filtered of step (6), use the deionized water wash filtrate, 100 ℃ of-150 ℃ of oven dry, the 60-100 mesh sieve is crossed in 500 ℃-750 ℃ calcinings after 20-30 minute, get product.
5. the preparation method of multi-layer multi-color changing colour change interval pigment as claimed in claim 4 is characterized in that specific refractory power is a chlorate greater than the solubility inorganic metal salt of 2.0 oxide compound correspondence, as SnCl
4Or TiCl
4Or FeCl
3Specific refractory power less than the soluble inorganic salt of 1.8 oxide compound correspondence is: Na
2SiO
3Or AlCl
3Or Na
2B
4O
7
6. multi-layer multi-color changing colour change interval pigment according to claim 1 is mainly used in industries such as coating, printing ink, makeup, leather, plastic and glass.
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