CN103911023B - Optical color and preparation method thereof - Google Patents

Optical color and preparation method thereof Download PDF

Info

Publication number
CN103911023B
CN103911023B CN201310006609.5A CN201310006609A CN103911023B CN 103911023 B CN103911023 B CN 103911023B CN 201310006609 A CN201310006609 A CN 201310006609A CN 103911023 B CN103911023 B CN 103911023B
Authority
CN
China
Prior art keywords
optical color
oxide
substrate
silica
clad
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310006609.5A
Other languages
Chinese (zh)
Other versions
CN103911023A (en
Inventor
付建生
张军礼
刘越
刘挺
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Longhua New Material Co., Ltd
Original Assignee
LONGHUA PEARLY-LUSTRE PIGMENT Co Ltd SHANTOU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LONGHUA PEARLY-LUSTRE PIGMENT Co Ltd SHANTOU filed Critical LONGHUA PEARLY-LUSTRE PIGMENT Co Ltd SHANTOU
Priority to CN201310006609.5A priority Critical patent/CN103911023B/en
Publication of CN103911023A publication Critical patent/CN103911023A/en
Application granted granted Critical
Publication of CN103911023B publication Critical patent/CN103911023B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The present invention is that, on a kind of optical color, the optical color includes substrate and the clad being coated on the substrate, wherein being at least coated with three kinds of coatings on described substrate successively, three kinds of described coatings are selected from successively:Titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, zirconium dioxide, chrome green or their mixture or compound;Silica;Alundum (Al2O3), bismuth oxide or their mixture or compound.The optical color that the present invention is provided is overcome in the prior art because pigment particles are small, so that particle diameter reflecting surface is small, the low defect of the saturation degree of color.Simultaneously, the invention further relates to a kind of preparation method of optical color, the preparation method overcomes the defect of clad " lamination " in the prior art, while reducing the covering amount of clad, add the number of particles in Unit Weight so that the paint color of preparation is fuller and rich and changeful.

Description

Optical color and preparation method thereof
Technical field
The present invention relates to a kind of product for fields such as ceramics, cosmetics, coating, printing, plastics, speciality paper, chemical industry, A kind of more particularly to optical color for above-mentioned field.Further, the invention further relates to the system of above-mentioned optical color Preparation Method.
Background technology
Interference colours pearlescent pigment is characterized in the one or more gold of the laminar one or many claddings of substrate surface Belong to oxide, by multiple refraction, reflection and transmission of the visible ray on metal oxide and substrate interface, wrapped by adjustment The geometric thickness or optical thickness of the metal oxide covered, make pigment particles surface form the interference of light so that pigment particles have There are interference colours, and assign product with color.This color makes one to feel there is depth, so that with the general light of similar pearl Pool.
In order to beautify the life of people, people develop discoloration pearlescent pigment again, when object applies this pigment, such as use In the high plastics PP of the transparency(Polypropylene)Or PS(Polystyrene), when people observe object from different perspectives, it has difference Color, while these colors have very high color saturation.Make object that there is very magical sensation.
Discoloration pearlescent pigment is structurally characterized in that, in the Surface coating multilevel oxide of substrate, and these oxide structures It is the high structure of height, i.e., first in the floor height index metal oxide of Surface coating one of substrate, then coats one layer of low-refraction gold Belong to oxide, then coat high refractive index metal oxide.By changing the thickness that each layer is coated, the color for obtaining different range becomes Change.Its concrete structure is:
Substrate/high refractive index metal oxide/low-refraction oxide/high refractive index metal oxide
The substrate for being generally used for discoloration pearlescent pigment is mica(Crystalline state), sheet glass(Amorphous state)With oxidation iron plate(It is brilliant State).And the metal oxide for being used for high refractive index layer is usually used titanium oxide, iron oxide and iron titanate, and it is used for low folding The oxide for penetrating rate layer is aluminum oxide and silica or their mixture, other low refractions can be also contained certainly saturating Bright oxide.
Low-refraction oxide is prepared or constituted by the compound of low-refraction in this structure, usually titanium dioxide Silicon, and this silicon dioxide layer be it is unbodied, it is amorphous.Other compounds are rarely seen so far using wet chemistry method hydrolysis precipitation Report.
High refractive index metal oxide is usually titanium dioxide or/and iron oxide in this structure, and they are crystalline state, such as sharp Titanium ore type titanium dioxide, rutile titanium dioxide, α-di-iron trioxide etc..
There are problems that during such discoloration pearlescent pigment, one is as pigment particles particle diameter diminishes, due to Unit Weight Particle seamed edge increase, the thickness of low-refraction clad is still very thick so that pigment particles reflectivity reduce, and Scattered power increase, so that the interference of light of pigment dies down, the saturation degree reduction of interference colours.
When preparing such discoloration pearlescent pigment, it is easy to " lamination " phenomenon occur during hydrolysis cladding silica, especially When using particle diameter very little, radius-thickness ratio very big mica when be particularly acute, it is scattered in coating that this lamination will result in pigment The saturation degree degradation of problem, glossiness and color, simultaneously because fine particle size reflecting surface itself is with regard to small, the saturation degree of color It is just low, so that the application of small particle camouflage paint loses use value.
As discoloration pearlescent pigment is applied to printing-ink field, and require that pigment particle size is smaller, while needing into one Step improve pigment color saturation, allow for solve these problems become more urgent.
In addition, also a kind of superpower interference colours pearlescent pigment, it is to coat different metal oxides in substrate surface, is formed " height is high " refractive index structures, this structure is similar to discoloration pearlescent pigment, only low-refraction oxide(It is usually amorphous Silica)Covering amount is fewer, does not reach the optical thickness required for discoloration, but due to its presence, can greatly improve The saturation degree of interference colours, i.e., commonly called strong interference colours pearlescent pigment.
As can be seen here, above-mentioned existing pearlescent pigment is in performance and application field, it is clear that still suffer from some defects, and urgently Wait to be further improved.The present inventor is known based on such product design manufacture abundant for many years practical experience and specialty is engaged in Know, and coordinate the utilization of scientific principle, be actively subject to research and innovation, to found a kind of new optical color and preparation method thereof, energy It is enough to improve the defect that general existing pearlescent pigment is present, it is had more practicality.By constantly research, design, and through anti- After retrial is made and improved, the present invention having practical value is created finally.
The content of the invention
It is a primary object of the present invention to, the defect for overcoming existing pearlescent pigment to exist, and a kind of new optics is provided Pigment, technical problem to be solved be overcome pigment particles become hour produced by pigment particles reflectivity reduce and dissipate Rate increase is penetrated, so that the interference of light of pigment dies down, the defect of the saturation degree of interference colours reduction, so that the present invention is more Suitable for practicality, and with the value in industry.
Another object of the present invention is to there is provided a kind of preparation method of optical color, technical problem to be solved: When preparing such discoloration pearlescent pigment, hydrolysis cladding clad when be easy to " lamination " phenomenon occur, especially when using grain Footpath very little, radius-thickness ratio very big mica when be particularly acute, this lamination will result in scattering problem of the pigment in coating, gloss The saturation degree degradation of degree and color, simultaneously because fine particle size reflecting surface itself is just small, the saturation degree of color is just low, thus So that the application of small particle camouflage paint loses use value.
The object of the invention to solve the technical problems is realized using following technical scheme.According to present invention proposition A kind of optical color, the optical color includes substrate and the clad that is coated on the substrate.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
Foregoing optical color, wherein the material of described substrate be selected from phyllosilicate, glass flake, flake ferric oxide, Tabular alumina or bismoclite chip.
Foregoing optical color and preparation method thereof, wherein described phyllosilicate is natural mica powder or synthetic mica Powder.
Foregoing optical color, wherein the material of described clad is selected from alundum (Al2O3), aluminium hydroxide, aqua oxidation One or more in aluminium, titanium dioxide, di-iron trioxide, iron hydroxide or silica.
Foregoing optical color, wherein the particle diameter of described substrate is 5-1500 microns, the particle diameter and thickness of the substrate Than more than or equal to 60.
Foregoing optical color, wherein being comprised at least in described clad has silica.
Foregoing optical color, wherein described silica is amorphous state or unbodied.
Foregoing optical color, wherein containing dopant in described silica, described dopant is selected from three oxidations Two aluminium, aluminium hydroxide, titanium dioxide, di-iron trioxide, iron hydroxide or their mixture.
Foregoing optical color, wherein the weight of described dopant is the 0.01~40% of the silica weight.
Foregoing optical color, wherein the weight of described dopant is the 4~25% of the silica layer weight.
Foregoing optical color, wherein described clad, which is further included, is selected from alundum (Al2O3), aluminium hydroxide, hydration Two or more in aluminum oxide, titanium dioxide, di-iron trioxide or iron hydroxide.
Foregoing optical color, wherein three kinds of coatings are at least coated with described substrate successively, three kinds of described bags Thing is covered to be selected from successively:Titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, titanium dioxide Zirconium, chrome green or their mixture or compound;Silica;Alundum (Al2O3), bismuth oxide or theirs is mixed Compound or compound.
Foregoing optical color, wherein described substrate is before other coatings are coated, first coated silica, three oxygen Change two aluminium, bismuth oxide or their mixture or compound.
Foregoing optical color, wherein the material of described substrate be selected from phyllosilicate, glass flake, flake ferric oxide, Tabular alumina or bismoclite chip.
Foregoing optical color, wherein described phyllosilicate is natural mica powder or compound mica.
Foregoing optical color, wherein the particle diameter of described substrate is 5-1500 microns, the particle diameter and thickness of the substrate Than more than or equal to 60.
Foregoing optical color, wherein described silica is amorphous state or unbodied.
Foregoing optical color, wherein containing dopant in described silica, described dopant is selected from three oxidations Two aluminium, aluminium hydroxide, titanium dioxide, di-iron trioxide, iron hydroxide or their mixture.
Foregoing optical color, wherein the weight of described dopant is the 0.01~40% of the silica weight.
Foregoing optical color, wherein the weight of described dopant is the 4~25% of the silica layer weight.
Foregoing optical color, wherein being further provided with protective layer on described clad.
The object of the invention to solve the technical problems is also realized using following technical scheme.According to present invention proposition A kind of method for preparing optical color, this method comprises the following steps:
Substrate and appropriate pure water are stirred and to form kettle liquid;
Add one or more of soluble-salt aqueous hydrolysis claddings;
Filtering, washing, drying and calcining.
The preparation method of foregoing optical color, wherein the step of further comprising the temperature and the pH that adjust kettle liquid.
The preparation method of foregoing optical color, wherein the temperature of the kettle liquid after described adjustment is 60-85 DEG C, it is described PH value is 1-10.
The preparation method of foregoing optical color, wherein adding one or more of soluble-salt aqueous hydrolysis claddings Before, pH value is adjusted to by 1.5-9.0 by the appropriate acid of addition.
The preparation method of foregoing optical color, wherein described one or more of soluble salt solutions, which are selected from, can generate two Titanium oxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, zirconium dioxide, chrome green or Their mixture or compound;Silica;The nothing of alundum (Al2O3), bismuth oxide or their mixture or compound Machine salt.
The present invention has clear advantage and beneficial effect compared with prior art.From above technical scheme, in order to Aforementioned invention purpose is reached, main technical content of the invention is as follows:
Optical color realizes that discoloration can have a various structures, the clad and current pearlescent pigment of optical color of the invention Employed in clad be different.
In one embodiment of this invention, the clad in optical color is the compound by different refractivity according to certain Ratio and method mixing after formed.
In one embodiment of this invention, the oxide mixed in amorphous silicon di-oxide is optional so that in amorphous In state silica separately or concurrently containing alundum (Al2O3), aluminium hydroxide, hydrated alumina, titanium dioxide, di-iron trioxide, Iron hydroxide etc., these oxides are uniformly present in dots in amorphous amorphous silicon di-oxide layer so that this two Silicon oxide layer is changed into a heterogeneous layer, i.e., both there is continuous phase amorphous silicon di-oxide, and there is also the height refraction of spot distribution Rate or low-refraction oxide fine particle.Wherein, so-called high or low refractive index right and wrong crystalline silicon dioxide is Comparatively speaking.Higher than nothing Amorphous silicon dioxide refractive index for high index of refraction, be low-refraction material less than amorphous silica refractive index, with profit In defining.
In another embodiment of the invention, the oxide fine particle being present in amorphous silicon di-oxide layer is with " point " Form is uniformly distributed;Oxide fine particle can also be such as high as needed along the regular distribution in direction perpendicular to this unformed layer The density of index oxides particulate from less to more, or from more to less, or completely the same, or according to a certain functional relation point Cloth, to obtain different or required optics and property and effect.
It is present in the particle diameter of the oxide fine particle in amorphous silicon di-oxide layer, usually several nanometers, preferably 1-10 Nanometer, particularly preferably 5 rans.
The oxide fine particle being present in amorphous silicon di-oxide layer can be amorphous or crystalline state, such as Titanium dioxide is typically crystalline state, and di-iron trioxide is typically crystalline state.
The oxide fine particle being present in amorphous silicon di-oxide layer can be oxide or hydrous oxide, Can also be hydroxide or some basic metal salt.
The content for being present in the high index oxide fine particle in low-refraction amorphous silicon di-oxide layer is preferably 0.01-40%, particularly preferably 4-25%.
The refractive index for being present in the oxide fine particle in amorphous silicon di-oxide layer is greater than amorphous silicon di-oxide refraction All metals and/or nonmetal oxide of rate.
The refractive index for being present in the oxide fine particle in amorphous silicon di-oxide layer is less than amorphous silicon di-oxide refraction All metals and/or nonmetal oxide of rate.
Through from the foregoing, invention is on a kind of optical color, the optical color includes substrate and cladding Clad on the substrate, wherein three kinds of coatings are at least coated with described substrate successively, three kinds of described coatings It is selected from successively:Titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, zirconium dioxide, Chrome green or their mixture or compound;Silica;Alundum (Al2O3), bismuth oxide or their mixture Or compound.The optical color that the present invention is provided is overcome in the prior art because pigment particles are small, so that particle diameter reflecting surface is small, The low defect of the saturation degree of color.Meanwhile, the invention further relates to a kind of preparation method of optical color, the preparation method overcomes The defect of clad " lamination ", while reducing the covering amount of clad, adds the particle in Unit Weight in the prior art Quantity so that the paint color of preparation is fuller and rich and changeful.
Heretofore described substrate specification is preferably radius-thickness ratio >=60, and radius-thickness ratio is the bigger the better, the definition of radius-thickness ratio:Footpath The thickness of the diameter of thickness rate=substrate particle/substrate particle
Optical color of the present invention wherein further comprises provided with post processing cladding nitride layer on described oxide coating, With suitable for specific use(Weather-proof clad during such as outdoor applications).
By above-mentioned technical proposal, optical color of the present invention and preparation method thereof at least has following advantages:
(1)Due to containing oxide in amorphous silicon di-oxide layer, make the amorphous state titanium dioxide when preparing camouflage paint The thickness of silicon layer decreases, so that the thickness of whole finished pigment is reduced, and can be used and prepares color compared with small particle substrate and satisfy The higher color-change optical pigment with degree, more preferably, the consumption of pigment is reduced covering power, use cost reduction.
(2)The process for preparing amorphous silicon di-oxide clad is to use wet-chemical hydrolytic precipitation, due to there is oxide micro- Grain forms be co-deposited together, is thus not likely to produce " lamination " phenomenon, so that finished pigment particle is single presence, can Color effect, and optimum dispersion effect are played to greatest extent.Be conducive to preparing compared with small particle camouflage paint.
In summary, special optical color of the present invention and preparation method thereof, it has the advantages that above-mentioned many and practicality Value, and publish or use in the like product design similar with there are no in preparation method and really belong to innovation, it is in work( Can on all have larger improvement, technically have large improvement, and generate handy and practical effect, and compared with prior art Multinomial effect with enhancement, thus more suitable for practicality, and the extensive value with industry, really for it is one novel, progressive, Practical new design.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
The high power transmission electron microscope of optical color of the present invention is shown in Fig. 1(HTEM)Figure, wherein(A)For amorphous state Crystalline titania in silica,(B)For the crystalline state iron oxide layer coated on amorphous silicon di-oxide.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with Accompanying drawing and preferred embodiment, to according to optical color proposed by the present invention and preparation method thereof its embodiment, step, knot Structure, feature and its effect, are described in detail as after.
Embodiment 1
This example demonstrates that how optical color of the present invention is prepared.
A certain amount of substrate is put into reactor, and adds appropriate pure water, stirs and is warming up to 70-80 DEG C, use Kettle liquid is adjusted to a certain pH value by acid or alkali lye, then with the high index of refraction metal salt of certain metered a certain concentration of speed Solution(Such as titanium tetrachloride or ferric trichloride), while being added dropwise to alkali lye to maintain the pH value of kettle liquid, when coating a certain interference colours, stop Only feed;The pH value of alkali lye rise kettle liquid is slow added into 8-9, then with the water glass of the metered a certain concentration of a certain speed Glass solution, while with the metered metal salt of a certain speed(The dissolvable metal salt of high refractive index oxide can be generated)It is water-soluble Liquid, this charging rate can be varied as desired in, then add watery hydrochloric acid simultaneously to maintain the pH value of kettle liquid, after adding, then use The pH value of kettle liquid is slowly lowered to when continuing to increase reflective metal salting liquid by watery hydrochloric acid, then with certain speed metering plus Enter the high index of refraction metal salt solution of a certain concentration(Such as titanium tetrachloride or ferric trichloride), while being added dropwise to alkali lye to maintain kettle liquid PH value, coat a certain interference colours when, stop charging.Filtering, uses pure water desalination, dries, then is calcined with certain temperature, i.e., Obtain required product.
Substrate in the present embodiment is selected from:Natural mica, synthetic mica, sheet glass, flake ferric oxide, tabular alumina or One or more in bismoclite chip.
The clad on substrate in the present embodiment be followed successively by titanium dioxide, the amorphous silicon di-oxide containing iron oxide, Bismuth oxide.
In the present embodiment, the top layer of optical color can further contain layer protective layer.
In the present embodiment, the amorphous silicon di-oxide containing oxide particle can be layered repeatedly to go out in optical color It is existing, and successively coated by other oxide skin(coating)s.
Embodiment 2
The present embodiment further illustrates how optical color of the present invention is prepared.
A certain amount of substrate is put into reactor, and adds appropriate pure water, stirs and is warming up to 70-80 DEG C, use The pH value of kettle liquid is transferred to 8-9 by alkali lye, is then slowly dropped into a certain amount of water glass solution with certain speed, while being added dropwise to acid solution To safeguard that the pH value of kettle liquid is constant, after adding, kettle liquid is adjusted to a certain pH value with acid solution, then added with certain speed metering Enter the high index of refraction metal salt solution of a certain concentration(Such as titanium tetrachloride or ferric trichloride), while being added dropwise to alkali lye to maintain kettle liquid PH value, coat a certain interference colours when, stop charging;The pH value of alkali lye rise kettle liquid is slow added into 8-9, then with a certain The water glass solution of the metered a certain concentration of speed, while with the metered metal salt of a certain speed(High index of refraction can be generated The dissolvable metal salt of oxide)The aqueous solution, this charging rate can be varied as desired in, then add watery hydrochloric acid simultaneously to tie up The pH value of kettle liquid is held, after adding, then slowly the pH value of kettle liquid is lowered to watery hydrochloric acid continues to increase reflective metal salting liquid When, then with the high index of refraction metal salt solution of certain metered a certain concentration of speed(Such as titanium tetrachloride or tri-chlorination Iron), while being added dropwise to alkali lye to maintain the pH value of kettle liquid, when coating a certain interference colours, stop charging.Filtering, uses pure water Desalination, drying, then calcined with certain temperature, that is, obtain required product.
The structure for the product being made up of the present embodiment is substrate/E layers/A layers/B layers/C layers/D layers;Wherein:
E layers:Amorphous silicon di-oxide thin layer;
A layers:Titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, titanium dioxide Zirconium, chrome green or their mixture or compound;
B layers:Amorphous silicon di-oxide, wherein be mixed with titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, Cobalt oxide, cobalt sesquioxide, zirconium dioxide, chrome green, alundum (Al2O3) or bismuth oxide;
C layers:Alundum (Al2O3) or bismuth oxide;
D layers are:External protection, this layer is coated as needed.
In the present embodiment, the structure for the new construction optical color being made can also be substrate/E layers/A layers/B as needed Layer/C layers/B layers/C layers/D layers.Wherein A, B, C and D are as described above.Acid wherein used is hydrochloric acid or sulfuric acid, hydroxide used Sodium, potassium hydroxide, ammonium hydroxide.
Embodiment 3
It is substrate by the compound mica that 100 gram particle footpaths are 10-60 microns, and puts into 2000 milliliters of reactor, Stirring is warming up to 75 DEG C, uses hydrochloric acid(30%)Kettle liquid pH value is transferred to 3.2, tri-chlorination is then added dropwise with 30 mls/hour of speed Ferrous solution(100g(FeCl3)/L), while sodium hydroxide solution is added dropwise(NaOH, 15%)To maintain pH constant, until substrate interference Color is light yellow, then uses sodium hydroxide solution(NaOH, 15%)The pH of kettle liquid is transferred to 9, then with 30 mls/hour of speed Water glass solution is added dropwise(30g(SiO2)/L), while titanium tetrachloride solution is added dropwise(200g(TiCl4)/L), drop rate makes dioxy The ratio between SiClx and titanium dioxide are 100:12, while hydrochloric acid solution is added dropwise(30%)To maintain the pH of kettle liquid constant, until substrate reaches To interference colours green, then use hydrochloric acid solution(30%)The pH value of kettle liquid is lowered to 3.2, then dripped with 30 mls/hour of speed Plus liquor ferri trichloridi(100g(FeCl3)/L), while sodium hydroxide solution is added dropwise(NaOH, 15%)To maintain pH constant, until Substrate interference colours are reddish violet.
Then filter, with pure water, with 120 DEG C of drying, calcine 450 DEG C, and be incubated 30 minutes.Products obtained therefrom be with The red green color-change optical pigment of higher saturated color.
It refer to Fig. 1 HTEM, it can be seen that in amorphous silicon di-oxide layer, contain more crystalline titania grain Son, its particle diameter is general in 5 rans, and in than relatively evenly, with the formal distribution of " dot matrix " in amorphous titanium dioxide In silicon layer.And outermost layer can also clearly see hematite layer, and this hematite layer is crystalline state.Titanium dioxide The lattice parameter of titanium and di-iron trioxide is substantially as shown in Figure 1.
Embodiment 4
It is substrate by the compound mica that 100 gram particle footpaths are 10-60 microns, and puts into 2000 milliliters of reactor, Stirring is warming up to 75 DEG C, uses alkali lye(NaOH, 15%)The pH value of kettle liquid is transferred to 9, water glass solution is then added dropwise to(30g (SiO2)/L)30 milliliters, while hydrochloric acid is added dropwise(30%)Maintain the pH value of kettle liquid constant, hydrochloric acid is then added dropwise(30%)By kettle liquid pH Value is transferred to 3.2, and liquor ferri trichloridi then is added dropwise with 30 mls/hour of speed(100g(FeCl3)/L), while hydrogen-oxygen is added dropwise Change sodium solution(NaOH, 15%)To maintain pH constant, until substrate interference colours is light yellow, then sodium hydroxide solution is used(NaOH, 15%)The pH of kettle liquid is transferred to 9, water glass solution is then added dropwise with 30 mls/hour of speed(30g(SiO2)/L), drip simultaneously Plus titanium tetrachloride solution(200g(TiCl4)/L), drop rate makes the ratio between silica and titanium dioxide be 100:12, drip simultaneously Plus hydrochloric acid solution(30%)To maintain the pH of kettle liquid constant, until substrate reaches interference colours green, then hydrochloric acid solution is used(30%)Will The pH value of kettle liquid is lowered to 3.2, and liquor ferri trichloridi then is added dropwise with 30 mls/hour of speed(100g(FeCl3)/L), together When sodium hydroxide solution is added dropwise(NaOH, 15%)To maintain pH constant, until substrate interference colours are reddish violet.
Then filter, with pure water, with 120 DEG C of drying, calcine 450 DEG C, and be incubated 30 minutes.Products obtained therefrom be with The red green color-change optical pigment of high saturated color.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people Member, without departing from the scope of the present invention, when method and technology contents using the disclosure above make it is a little more Equivalent embodiment that is dynamic or being modified to equivalent variations, as long as being the content without departing from technical solution of the present invention, according to the present invention's Any simple modification, equivalent variations and modification that technical spirit is made to above example, still fall within technical solution of the present invention In the range of.

Claims (15)

1. a kind of optical color, the optical color includes substrate and the clad being coated on the substrate, wherein described cladding Layer is at least coated with three kinds of coatings successively, and three kinds of described coatings are selected from successively:The clad of high index of refraction, selected from dioxy Change titanium, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, zirconium dioxide, chrome green or it Mixture or compound;Silica;The clad of low-refraction, selected from alundum (Al2O3), bismuth oxide or they Mixture or compound;Wherein described silica is amorphous state or unbodied;Contain in described silica and mix Debris, described dopant be selected from alundum (Al2O3), aluminium hydroxide, titanium dioxide, di-iron trioxide, iron hydroxide or they Mixture.
2. optical color according to claim 1, wherein the material of described substrate be selected from phyllosilicate, glass flake, Flake ferric oxide, tabular alumina or bismoclite chip.
3. optical color according to claim 2, wherein described phyllosilicate is natural mica powder or compound mica.
4. optical color according to claim 1, wherein the particle diameter of described substrate is 5-1500 microns, the substrate Particle diameter and thickness ratio be more than or equal to 60.
5. optical color according to claim 1, wherein the particle diameter of described substrate is 10-150 microns, the substrate Particle diameter and thickness ratio be more than or equal to 100.
6. optical color according to claim 1, wherein the weight of described dopant is the silica weight 0.01~40%.
7. optical color according to claim 6, wherein the weight of described dopant is the silica layer weight 4~25%.
8. optical color according to claim 1, wherein described clad, which is further included, is selected from alundum (Al2O3), hydrogen Two or more in aluminum oxide, hydrated alumina, titanium dioxide, di-iron trioxide or iron hydroxide.
9. optical color according to claim 1, wherein described substrate first coats two before other coatings are coated Silica, alundum (Al2O3), bismuth oxide or their mixture or compound.
10. optical color according to claim 1, wherein being further provided with protective layer on described clad.
11. a kind of method for preparing the optical color in claim 1~10 described in any claim, this method includes following Step:
Substrate and appropriate pure water are stirred and to form kettle liquid;
Add one or more of soluble-salt aqueous hydrolysis claddings;
Filtering, washing, drying and calcining.
12. preparation method according to claim 11, wherein the step of further comprising the temperature and the pH that adjust kettle liquid.
13. preparation method according to claim 12, wherein the temperature of the kettle liquid after described adjustment is 60-85 DEG C, institute The pH value stated is 1-10.
14. the preparation method according to claim 11 or 12, wherein adding one or more of soluble-salt aqueous solution water Before solution cladding, by adding, pH value is adjusted to 1.5-9.0 by appropriate acid.
15. preparation method according to claim 11, can give birth to wherein described one or more of soluble salt solutions are selected from Into titanium dioxide, tin ash, di-iron trioxide, ferroso-ferric oxide, cobalt oxide, cobalt sesquioxide, zirconium dioxide, three oxidations two Chromium or their mixture or compound;Silica;Alundum (Al2O3), bismuth oxide or their mixture or compound Inorganic salts.
CN201310006609.5A 2013-01-08 2013-01-08 Optical color and preparation method thereof Active CN103911023B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310006609.5A CN103911023B (en) 2013-01-08 2013-01-08 Optical color and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310006609.5A CN103911023B (en) 2013-01-08 2013-01-08 Optical color and preparation method thereof

Publications (2)

Publication Number Publication Date
CN103911023A CN103911023A (en) 2014-07-09
CN103911023B true CN103911023B (en) 2017-09-05

Family

ID=51037042

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310006609.5A Active CN103911023B (en) 2013-01-08 2013-01-08 Optical color and preparation method thereof

Country Status (1)

Country Link
CN (1) CN103911023B (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IL257821B2 (en) 2015-09-03 2024-01-01 Tagra Biotechnologies Ltd Microcapsules encapsulating a reflective agent
CN108084743B (en) * 2018-02-01 2020-12-22 广西七色珠光材料股份有限公司 Rutile type high-color saturation interference color pearlescent pigment and preparation method thereof
CN109054456B (en) * 2018-07-12 2020-10-20 福建坤彩材料科技股份有限公司 Silver pearlescent pigment based on synthetic mica and preparation method and application thereof
CN109853067A (en) * 2019-03-01 2019-06-07 华东理工大学 A kind of preparation method of viscose rayon delustring titanium dioxide
CN112795208A (en) * 2020-12-01 2021-05-14 正太新材料科技有限责任公司 Preparation method of organic high-catalytic pearlescent pigment
CN112993069B (en) * 2021-02-08 2022-09-06 保定嘉盛光电科技股份有限公司 Transparent color-developing optical film layer and preparation method and application thereof
CN112987158B (en) * 2021-04-09 2022-03-18 广东晟铂纳新材料科技有限公司 Iron-based optically variable pigment and manufacturing method and application thereof
CN113563758B (en) * 2021-08-12 2022-11-18 浙江深奥科技有限公司 Special environment-friendly ink for photochromic wall sticker and preparation process thereof
CN115710434A (en) * 2022-11-15 2023-02-24 福建坤彩材料科技股份有限公司 White pearlescent pigment and preparation method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0940451B9 (en) * 1998-03-02 2003-02-19 Basf Aktiengesellschaft Brilliant goniochromatic pigments based on iron oxide platelets bearing multiple coatings
CN1597793A (en) * 2004-08-10 2005-03-23 汕头市龙华珠光颜料有限公司 Pigment of multi-gradition discolour at diffierent direction and production process thereof
CN1625344A (en) * 2002-02-01 2005-06-08 默克专利股份有限公司 Use of multi-layer pigments in the food and pharmaceutical industry
CN1903944A (en) * 2004-07-27 2007-01-31 默克专利股份有限公司 Multilayered interference pigments
CN101006140A (en) * 2004-08-13 2007-07-25 默克专利股份有限公司 Nacreous pigments
CN101200605A (en) * 2007-12-10 2008-06-18 河北欧克精细化工股份有限公司 Weather-resistant multiple-layer alteration paint and preparation method thereof
CN101565563A (en) * 2009-04-22 2009-10-28 汕头市龙华珠光颜料有限公司 Novel angle-dependent heterochromous light interference pigment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0940451B9 (en) * 1998-03-02 2003-02-19 Basf Aktiengesellschaft Brilliant goniochromatic pigments based on iron oxide platelets bearing multiple coatings
CN1625344A (en) * 2002-02-01 2005-06-08 默克专利股份有限公司 Use of multi-layer pigments in the food and pharmaceutical industry
CN1903944A (en) * 2004-07-27 2007-01-31 默克专利股份有限公司 Multilayered interference pigments
CN1597793A (en) * 2004-08-10 2005-03-23 汕头市龙华珠光颜料有限公司 Pigment of multi-gradition discolour at diffierent direction and production process thereof
CN101006140A (en) * 2004-08-13 2007-07-25 默克专利股份有限公司 Nacreous pigments
CN101200605A (en) * 2007-12-10 2008-06-18 河北欧克精细化工股份有限公司 Weather-resistant multiple-layer alteration paint and preparation method thereof
CN101565563A (en) * 2009-04-22 2009-10-28 汕头市龙华珠光颜料有限公司 Novel angle-dependent heterochromous light interference pigment

Also Published As

Publication number Publication date
CN103911023A (en) 2014-07-09

Similar Documents

Publication Publication Date Title
CN103911023B (en) Optical color and preparation method thereof
CA2971306C (en) Pearlescent pigments, process for producing them, and use of such pigments
US8066811B2 (en) Pigment having angle dependence of the interference colors and its production process
CN106536640B (en) Effect pigment
CN100482747C (en) Interference pigment with a high covering power
CN105542517B (en) White and interference colours dumb light sheet coated pigment and preparation method
CN104327552B (en) A kind of high temperature resistant pearlescent pigment and preparation method thereof
WO2011103713A1 (en) New flip-flop interference pigments
CN102492312B (en) High-saturation iron-series pigment and production method thereof
JP2008509068A (en) Multilayer discoloration pigment whose color varies depending on angle and method for producing the same
DE1467468A1 (en) Mica flake pigment
CN101289580A (en) Production process of super strength interference pearlylustre pigment
KR20100004252A (en) Method of manufacturing hematite platelets, hematite platelets and hematite platelets pigment fabricated using thereof
JP5535425B2 (en) Filler, method for producing the same, and cosmetics
CN105504889A (en) Gold-series low-glossiness laminated pigment and preparation method thereof
CN102660157B (en) Large-sized synthesized mica pearlescent pigment and preparation method thereof
CN103249782B (en) Brilliant black pigments
CN110573577B (en) Bright pigment, pigment-containing composition, and pigment-containing coated body
CN108084743B (en) Rutile type high-color saturation interference color pearlescent pigment and preparation method thereof
CN101189306A (en) Sparkle effect of unique particle size distribution
CN201971776U (en) Coarse-grain-diameter pearlescent pigment capable of being coated with metal oxides with high refractive index
JP4190174B2 (en) High iris color titanium oxide and its manufacturing method
CN105623316A (en) Iron-red-series low-gloss lamellar pigment and preparation method thereof
CN205635454U (en) Magnetic pearlescent pigment
CN2712932Y (en) Strongly flaring coloring materials

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CP01 Change in the name or title of a patent holder

Address after: 515021 Guangdong Province, Shantou city industrial zone or industry Shengping Road No. 15

Patentee after: Guangdong Longhua New Material Co., Ltd

Address before: 515021 Guangdong Province, Shantou city industrial zone or industry Shengping Road No. 15

Patentee before: SHANTOU LONGHUA PEARL LUSTRE PIGMENTS Co.,Ltd.

CP01 Change in the name or title of a patent holder