CN106380898A - Mica titanium golden pigment with blue effect and preparation method thereof - Google Patents
Mica titanium golden pigment with blue effect and preparation method thereof Download PDFInfo
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
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- C09C2200/403—Low molecular weight materials, e.g. fatty acids
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Abstract
The invention relates to the field of pearlescent pigments, and discloses a titanium dioxide coated mica golden pigment with a blue effect, which comprises a substrate, at least two cation layers and at least two pigment anion layers, wherein the substrate is an innermost layer, the surface of the substrate is coated with a first cation layer, the surface of the first cation layer is coated with a first pigment anion layer, then the cation layers and the pigment anion layers are alternately coated to construct a multilayer ordered structure, and the outermost layer is a pigment anion layer. The invention can construct nano-scale different layers of phthalocyanine pigment on the surface of mica titanium pearlescent pigment in a controllable way so as to improve the blue effect and visual effect of the surface of the pearlescent pigment, and the product is used in the fields of automobile industry, anti-counterfeiting identification, ornaments, printing ink and the like; the method has the advantages of controllable nanometer thickness, excellent blue effect, simple process, environmental protection, advancement and wide application prospect.
Description
Technical field
The present invention relates to pearlescent pigment field, more particularly, to a kind of mica titanium gold pigment with blue effect and its
Preparation method.
Background technology
Pearlescent pigment refers to there is nacreous dicoration pigment, and it is with Muscovitum, tabular quartz, tabular alumina or piece
Shape glass powder is base material, then the metal oxide transparent Film laminated of its Surface coating one floor height refractive index forms, and works as illumination
When being mapped to the smooth interface of Opacifying pigment, reflected light and refraction-reflected light can be produced, interfere generation between them a kind of three-dimensional
Feel strong pearly-lustre color.Pearlescent pigment is because its gloss is strong, good decorating effect, that nontoxic, fast light, heat-resisting, chemical stability is good etc. is excellent
Good characteristic, is all widely used in fields such as auto industry, plastic, printer's ink, decorative paint, artwork Ornaments.Full generation at present
The total output of boundary's mica titanium nacreous material crosses ten thousand tons, big 22～55 dollars/Kg of price of international market.Nacreous mica face at present
The preparation method of material mainly makes the metal salt solution of solubility using wet chemistry method, becomes the hydrogen of indissoluble by changing its pH value
Oxide fine particle is simultaneously covered in the surface of sheet mica, and drying, roasting process obtain pearlescent pigment product, using humidifying
Method prepares pearlescent pigment mainly several coating methods as follows：Plus alkali neutralisation, boil- ing hydrolysis, buffer agent method and sandwich bag
Cover method.
A kind of pearlescent pigment of metallic cover of Application No. 201410052600.21., described pearlescent pigment includes lamellar
Base material, its flat substrates surface is formed with multiple spaced titanium dioxide nano-rods, and described flat substrates have entirely
Roughness Rz DIN, between 5-500, each titanium dioxide nano-rod wherein said and described flat substrates all deposits multiple
Metallic, described metallic is silver.Pearlescent pigment produces cladding and mainly adopts this method at present, obtains surface layer structure
Than larger and controllability not, the uneven of surface lamella coating makes refraction-reflected light out photochromic very miscellaneous to thickness.Shen
Please be number for a kind of 2015101137504 bluish-green series pearlescent pigments, described pigment includes：1) base material；2) it is deposited on base material
SnO2+TiO2Clad；With 3) it is deposited on SnO2+TiO2Chromium zinc cobalt class blue pigment clad on clad；Wherein chromium zinc cobalt
Class blue pigment layer be made up of chromium oxide, zinc oxide, cobalt oxide and aluminium oxide or main by chromium oxide, zinc oxide, cobalt oxide and
Aluminium oxide forms.
With the continuous development of technology, more and more higher is required to the visual effect of product, should possess the spy of pearlescent pigment
Point, can improve the concavo-convex stereovision of decorative parts again, especially have more advantage in anti-fake material and application aspect.And Surface coating
Nano thickness control current method be difficult to.
Content of the invention
The present invention is directed to prior art media layer damage, thickness degree and the uncontrollable shortcoming of layer number, there is provided a kind of layer knot
A kind of mica titanium gold pigment with blue effect that structure is controlled, thickness degree is controlled and layer number is controlled.
In order to solve above-mentioned technical problem, the present invention is addressed by following technical proposals：
A kind of mica titanium gold pigment with blue effect, including base material, at least two-layer cationic layer and at least two-layer
Pigment anion layer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating the
One layer pigment anion layer, then cationic layer replace cladding with pigment anion layer, one layer of outermost is pigment anion layer,
Repeatedly construct multiple structure assembled layers, base material is that cat gold is titanium nacreous.
Preferably, the material of cationic layer is PAH (PAH), PDDA
One of or two kinds of combinations (PDDA).
Preferably, the material of pigment anion layer be copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops one of polysulfonate or
Two kinds of combinations.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:3～5 mass fraction is 30% hydrogen peroxide and sulphuric acid that mass fraction is 98%
Mixing, obtains mixed solution；Base material is immersed in mixed solution, embathes at 60～90 DEG C 20～40 minutes, spend after filtration
The post-drying of ionized water flushing；
Step 2, the base material processing through step one is immersed in titanate coupling agent and the mixed solution of saline solution,
Embathe at 25～30 DEG C 20～40 minutes, wash after filtration, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, embathes 30～50 at 25～30 DEG C
Filter after minute, wash, dry up, make cationic layer Surface coating monolayer pigment anion layer；
Step 4, in immersion saline solution, embathes at 25～30 DEG C 20～40 minutes, washs after filtration, make pigment cloudy from
Sub-layer surface coats monolayer cationic layer, and for mass fraction, the PAH being 2.5%, mass fraction are saline solution
One of 3.5% PDDA or two kinds of combinations；
Step 5, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, embathes 30～50 at 25～30 DEG C
Filter after minute, wash, dry up, make cationic layer Surface coating monolayer pigment anion layer.
Preferably, repeat step four after step 5, step 5 obtain multilayer coating structure nano thickness cationic layer and
Pigment anion layer, one layer of outermost is pigment anion layer.
Preferably, copper phthalein green grass or young crops sulfonate is copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops one of polysulfonate or two kinds of groups
Close.Copper phthalein green grass or young crops sulfonate is thick phthalocyanine blue oleum sulfonation gained.
Preferably, the consumption of titanate coupling agent is the 0.01～0.6% of substrate mass fraction.
Preferably, the consumption of saline solution is the 6～25% of substrate mass fraction.
Preferably, the consumption of copper phthalein green grass or young crops sulfonate is the 7～18% of substrate mass fraction.
The present invention, due to employing above technical scheme, has significant technique effect：The present invention passes through molecular self-assembling
The mica titanium gold pigment with blue effect of method preparation passes through the concentration control controlling PAH, PDDA and copper phthalein green grass or young crops sulfonate
Preparative layer thickness, such that it is able to produce the pearl effect of the blue effect of different depth.The Muscovitum with blue effect of the present invention
The preparation method of titanium color pigment, the Rotating fields that can overcome metal-oxide deposition process in prior art are uncontrollable, thickness
Spend the uncontrollable and uncontrollable difficult problem of layer number, can according to the special demands of different purposes be designed preparing different-thickness,
The pearlescent pigment of the different numbers of plies, can effectively strengthen the visual effect of product, make that decorative parts are concavo-convex to have levels, more third dimension with
Can identification, and the environmental friendly simple, production economy of this method is profitable.The Muscovitum titanium with blue effect of the present invention
Color pigment can apply to auto industry, anti-counterfeit paint, ornament, printer's ink etc. effect build, have wide variety of before
Scape.
Brief description
Fig. 1 is the structural representation of the embodiment of the present invention 1；
The toponym that in accompanying drawing, each number designation is referred to is as follows：1 base material, 2 ground floor cationic layers, 3
One layer pigment anion layer, 4 second layer cationic layers, 5 second layer pigment anion layers.
Specific embodiment
Example below is that the present invention is described in further detail, but is not to limit the scope of the present invention.
Embodiment 1
A kind of mica titanium gold pigment with blue effect, as shown in figure 1, include base material 1, two-layer cationic layer and two
Layer pigment anion layer, base material 1 is innermost layer, base material 1 Surface coating ground floor cationic layer 2, ground floor cationic layer 2 surface
Coat the first layer pigment anion layer 3, the first layer pigment anion layer 3 coats second layer cationic layer 4, second layer cationic layer
4 Surface coating the second layer pigment anion layers 5；Base material 1 is that cat gold is titanium nacreous, and the material of cationic layer is PAH, face
The material of material cationic layer is copper phthalein green grass or young crops polysulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:4 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；Base material 1 is immersed in mixed solution, embathes at 72 DEG C 32 minutes, obtain solid after filtration, spend
The post-drying of ionized water flushing；
Step 2, by the PAH that the base material 1 processing through step one immerses titanate coupling agent and mass fraction is 2.5%
Mixed solution in, the consumption of titanate coupling agent is the consumption of 0.05%, PAH of substrate mass fraction is substrate mass fraction
6%, embathe at 23 DEG C 40 minutes, filtration washing after taking-up, make base material 1 Surface coating ground floor cationic layer 2；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 16% of substrate mass fraction, embathe at 27 DEG C 30 minutes and filter afterwards, wash, drying up, make ground floor cationic layer 2 table
Bread covers the first layer pigment anion layer 3；
Step 4, immersion mass fraction is in 2.5% solution of PAH, and the consumption of PAH is substrate mass fraction
15%, embathe at 23 DEG C 40 minutes, wash after filtration, make the first layer pigment anion layer 3 Surface coating second layer cation
Layer 4；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 16% of substrate mass fraction, embathe at 27 DEG C 30 minutes and filter afterwards, wash, drying up, make second layer cationic layer 4 table
Bread covers the second layer pigment anion layer 5.
Embodiment 2
A kind of mica titanium gold pigment with blue effect, includings base material, two-layer cationic layer and two layer pigments the moon from
Sublayer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating the first layer pigment
Anion layer, the first layer pigment anion layer cladding second layer cationic layer, second layer cationic layer Surface coating second layer face
Material anion layer, base material is that cat gold is titanium nacreous, and the material of cationic layer is PDDA, and the material of pigment cationic layer is
Copper phthalein green grass or young crops disulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:3 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 63 DEG C 28 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, by the PDDA that the base material processing through step one immerses titanate coupling agent and mass fraction is 3.5%
Mixed solution in, the consumption of titanate coupling agent is the consumption of 0.3%, PDDA of substrate mass fraction is substrate mass fraction
25%, embathe at 30 DEG C 20 minutes, filtration washing after taking-up, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops disulfonate in 8.0% copper phthalein green grass or young crops disulfonate solution
For the 22% of substrate mass fraction, embathe at 28 DEG C 40 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 4, immersion mass fraction is in 3.5% solution of PDDA, and the consumption of PDDA is substrate mass fraction
25%, embathe at 30 DEG C 20 minutes, wash after filtration, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops disulfonate in 8.0% copper phthalein green grass or young crops disulfonate solution
For the 22% of substrate mass fraction, embathe at 28 DEG C 40 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer, obtains cationic layer and the pigment anion layer of two-layer cladding.
Embodiment 3
A kind of mica titanium gold pigment with blue effect, include base material, three layers of cationic layer and three layer pigments the moon from
Sublayer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating the first layer pigment
Anion layer, the first layer pigment anion layer coats second layer cationic layer, and then cationic layer is replaced with pigment anion layer
Cladding, one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, the material of cationic layer be PAH and
The combination of PDDA, the material of pigment cationic layer is copper phthalein green grass or young crops polysulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:5 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 86 DEG C 20 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, the base material processing through step one is immersed in titanate coupling agent and the mixed solution of saline solution, titanium
The consumption of acid esters coupling agent is the 0.18% of substrate mass fraction, and saline solution is 1 for volume ratio:1 mass fraction is 2.5%
The mixed solution of PAH and PDDA that mass fraction is 3.5%, the consumption of saline solution is the 25% of substrate mass fraction, at 30 DEG C
Under embathe 20 minutes, filtration washing after taking-up, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 12% of substrate mass fraction, embathe at 26 DEG C 50 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 4, in immersion saline solution, saline solution is 1 for volume ratio:1 mass fraction be 2.5% PAH and quality divide
The mixed solution of the PDDA for 3.5% for the number, the consumption of saline solution is the 25% of substrate mass fraction, embathes 20 points at 30 DEG C
Clock, washs after filtration, makes pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 12% of substrate mass fraction, embathe at 26 DEG C 50 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 6, after step 5, repeat step four, step 5 obtain three layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
Embodiment 4
A kind of mica titanium gold pigment with blue effect, include base material, three layers of cationic layer and three layer pigments the moon from
Sublayer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating the first layer pigment
Anion layer, the first layer pigment anion layer coats second layer cationic layer, and then cationic layer is replaced with pigment anion layer
Cladding, one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, and the material of cationic layer is PDDA,
The material of pigment cationic layer is copper phthalein green grass or young crops polysulfonate and the combination of copper phthalein green grass or young crops disulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:4 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 60 DEG C 36 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, by the PAH that the base material processing through step one immerses titanate coupling agent and mass fraction is 2.5%
In mixed solution, the consumption of titanate coupling agent is the consumption of 0.6%, PAH of substrate mass fraction is substrate mass fraction
14%, embathe at 25 DEG C 27 minutes, filtration washing after taking-up, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, and copper phthalein green grass or young crops sulfonate for mass ratio is
1:2 copper phthalein green grass or young crops polysulfonate and the combination of copper phthalein green grass or young crops disulfonate, the consumption of copper phthalein green grass or young crops sulfonate is substrate mass fraction
13%, embathe at 30 DEG C 36 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating monolayer pigment anion layer；
Step 4, immersion mass fraction is in 2.5% mixed solution of PAH, and the consumption of PAH is substrate mass fraction
14%, embathe at 25 DEG C 27 minutes, wash after filtration, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, and copper phthalein green grass or young crops sulfonate for mass ratio is
1:2 copper phthalein green grass or young crops polysulfonate and the combination of copper phthalein green grass or young crops disulfonate, the consumption of copper phthalein green grass or young crops sulfonate is substrate mass fraction
13%, embathe at 30 DEG C 36 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating monolayer pigment anion layer；
Step 6, after step 5, repeat step four, step 5 obtain three layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
Embodiment 5
A kind of mica titanium gold pigment with blue effect, as shown in figure 1, include base material, four layers of cationic layer and four
Layer pigment anion layer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer is cloudy with pigment
Sheath replaces cladding, and one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, the material of cationic layer
Expect for PDDA, the material of pigment cationic layer is copper phthalein green grass or young crops polysulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:5 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 70 DEG C 40 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, by the PDDA that the base material processing through step one immerses titanate coupling agent and mass fraction is 3.5%
Mixed solution in, the consumption of titanate coupling agent is that the consumption of 0.21%, PDDA of substrate mass fraction divides for substrate mass
The 10% of number, embathes 22 minutes, filtration washing after taking-up at 27 DEG C, makes substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 9% of substrate mass fraction, embathe at 28 DEG C 44 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating list
Layer pigment anion layer；
Step 4, immersion mass fraction is in 3.5% solution of PDDA, and the consumption of PDDA is substrate mass fraction
10%, embathe at 27 DEG C 22 minutes, wash after filtration, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 9% of substrate mass fraction, embathe at 28 DEG C 44 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating list
Layer pigment anion layer；
Step 6, after step 5, repeat step four, step 5 obtain four layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
Embodiment 6
A kind of mica titanium gold pigment with blue effect, as shown in figure 1, include base material, four layers of cationic layer and four
Layer pigment anion layer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer is cloudy with pigment
Sheath replaces cladding, and one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, the material of cationic layer
Expect the combination for PAH and PDDA, the material of pigment cationic layer is copper phthalein green grass or young crops polysulfonate and the combination of copper phthalein green grass or young crops disulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:3 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 90 DEG C 24 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, the base material processing through step one is immersed in titanate coupling agent and the mixed solution of saline solution, titanium
The consumption of acid esters coupling agent is the 0.1% of substrate mass fraction, and saline solution is 1 for volume ratio:2 mass fraction is 2.5%
PAH and the PDDA that mass fraction is 3.5%, the consumption of saline solution is base material
The 22% of mass fraction, embathes 35 minutes, filtration washing after taking-up at 22 DEG C, makes substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, and copper phthalein green grass or young crops sulfonate for mass ratio is
1:1 copper phthalein green grass or young crops polysulfonate layer and the combination of copper phthalein green grass or young crops disulfonate, the consumption of copper phthalein green grass or young crops sulfonate is substrate mass fraction
18%, embathe at 25 DEG C 32 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating monolayer pigment anion
Layer；
Step 4, in immersion saline solution, saline solution is 1 for volume ratio:2 mass fraction is 2.5% PAH
Hydrochlorate and the PDDA that mass fraction is 3.5%, the consumption of saline solution is substrate mass fraction
22%, embathe at 22 DEG C 35 minutes, wash after filtration, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, and copper phthalein green grass or young crops sulfonate for mass ratio is
1:1 copper phthalein green grass or young crops polysulfonate layer and the combination of copper phthalein green grass or young crops disulfonate, the consumption of copper phthalein green grass or young crops sulfonate is substrate mass fraction
18%, embathe at 25 DEG C 32 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating monolayer pigment anion
Layer；
Step 6, after step 5, repeat step four, step 5 obtain four layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
Embodiment 7
A kind of mica titanium gold pigment with blue effect, as shown in figure 1, include base material, five layers of cationic layer and five
Layer pigment anion layer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer is cloudy with pigment
Sheath replaces cladding, and one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, the material of cationic layer
Expect for PAH, the material of pigment cationic layer is copper phthalein green grass or young crops disulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:4 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 80 DEG C 30 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, by the PAH that the base material processing through step one immerses titanate coupling agent and mass fraction is 2.5%,
The consumption of titanate coupling agent is the consumption of 0.01%, PAH of substrate mass fraction is the 19% of substrate mass fraction, at 24 DEG C
Under embathe 32 minutes, after filtration wash, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops disulfonate in 8.0% copper phthalein green grass or young crops disulfonate solution
For the 15% of substrate mass fraction, embathe at 30 DEG C 47 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 4, immersion mass fraction is in 2.5% solution of PAH, and the consumption of PAH is substrate mass fraction
19%, embathe at 24 DEG C 32 minutes and wash after filtering, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops disulfonate in 8.0% copper phthalein green grass or young crops disulfonate solution
For the 15% of substrate mass fraction, embathe at 30 DEG C 47 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 6, after step 5, repeat step four, step 5 obtain five layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
Embodiment 8
A kind of mica titanium gold pigment with blue effect, as shown in figure 1, include base material, five layers of cationic layer and five
Layer pigment anion layer, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer Surface coating
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer is cloudy with pigment
Sheath replaces cladding, and one layer of outermost is pigment anion layer, and base material is that cat gold is titanium nacreous, the material of cationic layer
Expect for PDDA, the material of pigment cationic layer is copper phthalein green grass or young crops polysulfonate.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Step one, volume ratio is 1:5 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 78 DEG C 22 minutes, after filtration, obtain solid, spend from
The post-drying of sub- water flushing；
Step 2, by the PDDA that the base material processing through step one immerses titanate coupling agent and mass fraction is 3.5%
Mixed solution in, the consumption of titanate coupling agent is the consumption of 2.4%, PDDA of substrate mass fraction is substrate mass fraction
12%, embathe at 30 DEG C 30 minutes, filtration washing after taking-up, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 10% of substrate mass fraction, embathe at 25 DEG C 42 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 4, immersion mass fraction is in 3.5% solution of PDDA, and the consumption of PDDA is substrate mass fraction
12%, embathe at 30 DEG C 30 minutes, wash after filtration, make pigment anion layer Surface coating monolayer cationic layer；
Step 5, immersion mass fraction is the consumption of copper phthalein green grass or young crops polysulfonate in 8.0% copper phthalein green grass or young crops polysulfonate solution
For the 10% of substrate mass fraction, embathe at 25 DEG C 42 minutes and filter afterwards, wash, drying up, make cationic layer Surface coating
Monolayer pigment anion layer；
Step 6, after step 5, repeat step four, step 5 obtain five layers of cationic layer coating nano thickness and face
Material anion layer, one layer of outermost is pigment anion layer.
In a word, the foregoing is only presently preferred embodiments of the present invention, all equalizations made according to scope of the present invention patent
Change and modification, all should belong to the covering scope of patent of the present invention.
Claims (9)
1. a kind of mica titanium gold pigment with blue effect it is characterised in that：Including base material, at least two-layer cationic layer and
At least two layer pigment anion layers, base material is innermost layer, and substrate surface coats ground floor cationic layer, ground floor cationic layer table
Bread covers the first layer pigment anion layer, and then cationic layer replaces cladding with pigment anion layer, and one layer of outermost is pigment
Anion layer, base material is that cat gold is titanium nacreous.
2. a kind of mica titanium gold pigment with blue effect according to claim 1 it is characterised in that：Cationic layer
Material be one of PAH, PDDA or two kinds combination.
3. a kind of mica titanium gold pigment with blue effect according to claim 1 it is characterised in that：Pigment cloudy from
The material of sublayer is copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops one of polysulfonate or two kinds of combinations.
4. a kind of preparation method of the mica titanium gold pigment with blue effect is it is characterised in that comprise the following steps：
Step one, volume ratio is 1:3～5 mass fraction be 30% hydrogen peroxide and sulphuric acid that mass fraction is 98% mix
Close, obtain mixed solution；By base material immerse mixed solution in, embathe at 60～90 DEG C 20～40 minutes, spend after filtration from
The post-drying of sub- water flushing；
Step 2, the base material processing through step one is immersed in the mixed solution of titanate coupling agent and saline solution, 25～
Embathe at 30 DEG C 20～40 minutes, wash after filtration, make substrate surface coat monolayer cationic layer；
Step 3, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, embathes 30～50 minutes at 25～30 DEG C
Filter afterwards, wash, dry up, make cationic layer Surface coating monolayer pigment anion layer.
Step 4, in immersion saline solution, embathes at 25～30 DEG C 20～40 minutes, washs, make pigment anion layer after filtration
Surface coating monolayer cationic layer, for mass fraction, the PAH being 2.5%, mass fraction are saline solution
One of 3.5% PDDA or two kinds of combinations；
Step 5, immersion mass fraction is in 8.0% copper phthalein green grass or young crops sulfonate solution, embathes 30～50 minutes at 25～30 DEG C
Filter afterwards, wash, dry up, make cationic layer Surface coating monolayer pigment anion layer.
5. the preparation method of a kind of mica titanium gold pigment with blue effect according to claim 4, its feature exists
In：Repeat step four after step 5, step 5 obtain cationic layer and the pigment anion layer of multilayer coating structure, one layer of outermost
For pigment anion layer.
6. the preparation method of a kind of mica titanium gold pigment with blue effect according to claim 4, its feature exists
In：Copper phthalein green grass or young crops sulfonate is copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops one of polysulfonate or two kinds of combinations.
7. the preparation method of a kind of mica titanium gold pigment with blue effect according to claim 4, its feature exists
In：The consumption of titanate coupling agent is the 0.01～0.6% of substrate mass fraction.
8. the preparation method of a kind of mica titanium gold pigment with blue effect according to claim 4, its feature exists
In：The consumption of saline solution is the 6～25% of substrate mass fraction.
9. the preparation method of a kind of mica titanium gold pigment with blue effect according to claim 4, its feature exists
In：The consumption of copper phthalein green grass or young crops sulfonate is the 7～18% of substrate mass fraction.
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| WO2009133895A1 (en) * | 2008-05-02 | 2009-11-05 | ポーラ化成工業株式会社 | Titania fine-particle composite and compositons coantining the titania fine-particle composite |
| WO2013018828A1 (en) * | 2011-08-03 | 2013-02-07 | 堺化学工業株式会社 | Composite powder and method for producing same |
| CN104392767A (en) * | 2014-09-30 | 2015-03-04 | 中国科学院上海硅酸盐研究所 | Graphene-based conductive pearlescent pigment and preparation method thereof |
| CN105838115A (en) * | 2016-04-27 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene-based conductive pearlescent pigment |
| CN105860593A (en) * | 2016-04-08 | 2016-08-17 | 广东工业大学 | Composition capable of enhancing pearlescent effect of pearlescent pigment, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009133895A1 (en) * | 2008-05-02 | 2009-11-05 | ポーラ化成工業株式会社 | Titania fine-particle composite and compositons coantining the titania fine-particle composite |
| WO2013018828A1 (en) * | 2011-08-03 | 2013-02-07 | 堺化学工業株式会社 | Composite powder and method for producing same |
| CN104392767A (en) * | 2014-09-30 | 2015-03-04 | 中国科学院上海硅酸盐研究所 | Graphene-based conductive pearlescent pigment and preparation method thereof |
| CN105860593A (en) * | 2016-04-08 | 2016-08-17 | 广东工业大学 | Composition capable of enhancing pearlescent effect of pearlescent pigment, and preparation method and application thereof |
| CN105838115A (en) * | 2016-04-27 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for preparing graphene-based conductive pearlescent pigment |
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