CN106380898B - 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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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/402—Organic protective coating
- C09C2200/403—Low molecular weight materials, e.g. fatty acids
- C09C2200/404—Low molecular weight materials, e.g. fatty acids comprising additional functional groups, e.g. -NH2, -C=C- or -SO3
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- C09C2220/00—Methods of preparing the interference pigments
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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 the decorative pigment with pearly luster, it is with mica, tabular quartz, tabular alumina or piece
Shape glass powder be base material, then its surface coat a floor height refractive index metal oxide transparent Film laminated form, work as illumination
When being mapped to the smooth interface of Opacifying pigment, reflected light and refraction-reflected light can be generated, interferes between them and generates a kind of solid
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 widely used in fields such as auto industry, plastic products, printer's ink, decorative paint, artwork Ornaments.Current full generation
The total output of boundary's mica titanium nacreous material has crossed 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 soluble metal salt solution using wet chemistry method, becomes the hydrogen of indissoluble by changing its pH value
Oxide fine particle and the surface for being covered in sheet mica, drying, roasting process obtain pearlescent pigment product, using humidifying
Method, which prepares pearlescent pigment, mainly following several coating methods：Add alkali neutralisation, boil- ing hydrolysis, buffer method and sandwich bag
Cover method.
A kind of pearlescent pigment of metallic cover of Application No. 201410052600.21., the pearlescent pigment include sheet
Base material, multiple spaced titanium dioxide nano-rods are formed on sheet substrate surface, and the sheet substrate has complete
Roughness Rz DIN are between 5-500, wherein all being deposited on each described titanium dioxide nano-rod and the sheet substrate multiple
Metallic, the metallic are silver.The cladding of pearlescent pigment production at present mainly adopts this method, and obtains surface layer structure
Thickness is bigger and controllability is inadequate, and the uneven of surface lamella coating causes refraction-reflected light to come out photochromic very miscellaneous.Shen
Please be number for a kind of 2015101137504 bluish-green serial pearlescent pigments, the pigment includes：1) base material；2) deposit on base material
SnO2+TiO2Clad；With 3) be deposited on SnO2+TiO2Chromium zinc cobalt class blue pigment clad on clad；Wherein chromium zinc cobalt
Class blue pigment layer be made of chromium oxide, zinc oxide, cobalt oxide and aluminium oxide or mainly by chromium oxide, zinc oxide, cobalt oxide and
Aluminium oxide forms.
It is higher and higher to the visual effect requirement of product with the continuous development of technology, should possess the spy of pearlescent pigment
Point, and the concave-convex stereovision of decorative parts can be improved, especially advantage is had more in anti-fake material and application aspect.And surface coats
Nano thickness current method is controlled to be difficult to.
The content of the invention
The present invention provides a kind of layer of knot for prior art media layer damage, layer thickness and the uncontrollable shortcoming of layer number
A kind of mica titanium gold pigment with blue effect that structure is controllable, layer thickness is controllable and layer number is controllable.
In order to solve the 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 layers of cationic layer and at least two layers
Pigment anion layer, base material are innermost layer, substrate surface cladding first layer cationic layer, first layer cationic layer surface cladding the
One layer pigment anion layer, then cationic layer replace cladding with pigment anion layer, one layer of outermost is pigment anion layer,
Multilayered structure assembled layers are repeatedly constructed, base material is titanium nacreous for cat gold.
Preferably, the material of cationic layer is polyallylamine hydrochloride (PAH), polydimethyl diallyl ammonium chloride
One or both of (PDDA) combination.
Preferably, the material of pigment anion layer for copper phthalein green grass or young crops disulfonate, one kind in copper phthalein green grass or young crops polysulfonate or
Two kinds of combinations.
A kind of preparation method of the mica titanium gold pigment with blue effect, comprises the following steps：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 3~5 mass fraction is 30% are 98%
Mixing, obtains mixed solution；Base material is immersed in mixed solution, embathes at 60~90 DEG C 20~40 minutes, is spent after filtering
Ionized water is dried after rinsing；
Step 2 will be immersed through the processed base material of step 1 in the mixed solution of titanate coupling agent and salting liquid,
It embathes at 25~30 DEG C 20~40 minutes, is washed after filtering, substrate surface is made to coat individual layer cationic layer；
Step 3 immerses in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, embathes 30~50 at 25~30 DEG C
Filtering, washing, drying, make cationic layer surface coat monolayer pigment anion layer after minute；
Step 4, immerse salting liquid in, embathe at 25~30 DEG C 20~40 minutes, washed after filtering, make pigment the moon from
Sub-layer surface coat individual layer cationic layer, salting liquid be mass fraction be 2.5% polyallylamine hydrochloride, mass fraction be
The combination of one or both of 3.5% polydimethyl diallyl ammonium chloride；
Step 5 immerses in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, embathes 30~50 at 25~30 DEG C
Filtering, washing, drying, make cationic layer surface coat monolayer pigment anion layer after minute.
Preferably, step 5 after repeat Step 4: step 5 obtain multilayer coating structure nano thickness cationic layer and
Pigment anion layer, one layer of outermost are pigment anion layer.
Preferably, copper phthalein green grass or young crops sulfonate is one or both of copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops polysulfonate group
It closes.Copper phthalein green grass or young crops sulfonate is obtained by thick phthalocyanine blue oleum sulfonation.
Preferably, the dosage of titanate coupling agent is the 0.01~0.6% of substrate mass fraction.
Preferably, the dosage of salting liquid is the 6~25% of substrate mass fraction.
Preferably, the dosage of copper phthalein green grass or young crops sulfonate is the 7~18% of substrate mass fraction.
The present invention has significant technique effect as a result of above technical scheme：The present invention passes through molecular self-assembling
The mica titanium gold pigment for blue effect that prepared by method have is by controlling the concentration control of PAH, PDDA and copper phthalein green grass or young crops sulfonate
Preparative layer thickness, so as to generate the pearl effect of the blue effect of different depth.The mica with blue effect of the present invention
The preparation method of titanium color pigment, can overcome that the layer structure of metal oxide deposition method in the prior art is uncontrollable, thickness
Spend the uncontrollable problem of uncontrollable and layer number, can be designed according to the special demands of different purposes prepare different-thickness,
Different layers of pearlescent pigments can effectively enhance the visual effect of product, decorative parts bumps is made to have levels, more three-dimensional sense with
Can identification, and this method it is environmental friendly it is simple, production economy is profitable.The mica titanium with blue effect of the present invention
The effect that color pigment can be applied to auto industry, anti-counterfeit paint, ornament, printer's ink etc. is built, before widely applied
Scape.
Description of the drawings
Fig. 1 is the structure diagram of the embodiment of the present invention 1；
The toponym that each number designation is referred in attached drawing is as follows：1-base material, 2-first layer cationic layer, 3-the
One layer pigment anion layer, 4-second layer cationic layer, the 5-the second layer pigment anion layer.
Specific embodiment
Example below is that the present invention is described in further detail, but is not limited the scope of the invention.
Embodiment 1
A kind of mica titanium gold pigment with blue effect, as shown in Figure 1, including base material 1, two layers of cationic layer and two
Layer pigment anion layer, base material 1 are innermost layer, and 1 surface of base material coats first layer cationic layer 2,2 surface of first layer cationic layer
Coat the first layer pigment anion layer 3, the first layer pigment anion layer 3 cladding second layer cationic layer 4, second layer cationic layer
4 surfaces coat the second layer pigment anion layer 5；Base material 1 is titanium nacreous for cat gold, and the material of cationic layer is PAH, face
The material for expecting 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 4 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；Base material 1 is immersed in mixed solution, is embathed at 72 DEG C 32 minutes, solid is obtained after filtering, is spent
Ionized water is dried after rinsing；
Step 2, the PAH that titanate coupling agent will be immersed through the processed base material 1 of step 1 and mass fraction is 2.5%
Mixed solution in, the dosage that the dosage of titanate coupling agent is 0.05%, PAH of substrate mass fraction is substrate mass fraction
6%, embathed at 23 DEG C 40 minutes, filtration washing after taking-up, make 1 surface of base material cladding first layer cationic layer 2；
Step 3 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 16% of substrate mass fraction, filtering, washing, drying, make 2 table of first layer cationic layer after being embathed at 27 DEG C 30 minutes
Bread covers the first layer pigment anion layer 3；
Step 4 is immersed in the solution for the PAH that mass fraction is 2.5%, and the dosage of PAH is substrate mass fraction
15%, it embathes at 23 DEG C 40 minutes, is washed after filtering, make 3 surface of the first layer pigment anion layer cladding second layer cation
Layer 4；
Step 5 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 16% of substrate mass fraction, filtering, washing, drying, make 4 table of second layer cationic layer after being embathed at 27 DEG C 30 minutes
Bread covers the second layer pigment anion layer 5.
Embodiment 2
A kind of mica titanium gold pigment with blue effect, including base material, two layers of cationic layer and two layer pigment the moon from
Sublayer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats the first layer pigment
Anion layer, the first layer pigment anion layer cladding second layer cationic layer, second layer cationic layer surface cladding second layer face
Expect anion layer, base material is titanium nacreous for cat gold, 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 3 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 63 DEG C 28 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2, the PDDA that titanate coupling agent will be immersed through the processed base material of step 1 and mass fraction is 3.5%
Mixed solution in, the dosage that the dosage of titanate coupling agent is 0.3%, PDDA of substrate mass fraction is substrate mass fraction
25%, embathed at 30 DEG C 20 minutes, filtration washing after taking-up, make substrate surface coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops disulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops disulfonate
For the 22% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 28 DEG C 40 minutes
Monolayer pigment anion layer；
Step 4 is immersed in the solution for the PDDA that mass fraction is 3.5%, and the dosage of PDDA is substrate mass fraction
25%, it embathes at 30 DEG C 20 minutes, is washed after filtering, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops disulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops disulfonate
For the 22% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 28 DEG C 40 minutes
Monolayer pigment anion layer obtains the cationic layer and pigment anion layer of two layers of cladding.
Embodiment 3
A kind of mica titanium gold pigment with blue effect, including base material, three layers of cationic layer and three layer pigment the moon from
Sublayer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats the first layer pigment
Anion layer, the first layer pigment anion layer coat second layer cationic layer, and then cationic layer replaces with pigment anion layer
Cladding, one layer of outermost are pigment anion layer, and base material is titanium nacreous for cat gold, the material of cationic layer for 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 5 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 86 DEG C 20 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2 will be immersed through the processed base material of step 1 in the mixed solution of titanate coupling agent and salting liquid, titanium
The dosage of acid esters coupling agent is the 0.18% of substrate mass fraction, and salting liquid is that volume ratio is 1:1 mass fraction is 2.5%
PAH and mass fraction are the mixed solution of 3.5% PDDA, and the dosage of salting liquid is the 25% of substrate mass fraction, at 30 DEG C
Under embathe 20 minutes, filtration washing after taking-up, make substrate surface coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 12% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 26 DEG C 50 minutes
Monolayer pigment anion layer；
Step 4 is immersed in salting liquid, and salting liquid is that volume ratio is 1:The PAH and quality point that 1 mass fraction is 2.5%
Number is the mixed solution of 3.5% PDDA, and the dosage of salting liquid is the 25% of substrate mass fraction, and 20 points are embathed at 30 DEG C
Clock washs after filtering, and pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 12% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 26 DEG C 50 minutes
Monolayer pigment anion layer；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of three layers of cladding nano thickness
Expect anion layer, one layer of outermost is pigment anion layer.
Embodiment 4
A kind of mica titanium gold pigment with blue effect, including base material, three layers of cationic layer and three layer pigment the moon from
Sublayer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats the first layer pigment
Anion layer, the first layer pigment anion layer coat second layer cationic layer, and then cationic layer replaces with pigment anion layer
Cladding, one layer of outermost are pigment anion layer, and base material is titanium nacreous for cat gold, and the material of cationic layer is PDDA,
The material of pigment cationic layer is the combination of copper phthalein green grass or young crops polysulfonate and 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 4 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 60 DEG C 36 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2 will immerse titanate coupling agent and mass fraction for 2.5% PAH's through the processed base material of step 1
In mixed solution, the dosage that the dosage of titanate coupling agent is 0.6%, PAH of substrate mass fraction is substrate mass fraction
14%, it is embathed at 25 DEG C 27 minutes, filtration washing after taking-up, substrate surface is made to coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, and copper phthalein green grass or young crops sulfonate is that mass ratio is
1:The combination of 2 copper phthalein green grass or young crops polysulfonate and copper phthalein green grass or young crops disulfonate, the dosage of copper phthalein green grass or young crops sulfonate is substrate mass fraction
13%, filtering, washing, drying, make cationic layer surface coat monolayer pigment anion layer after being embathed at 30 DEG C 36 minutes；
Step 4 is immersed in the mixed solution for the PAH that mass fraction is 2.5%, and the dosage of PAH is substrate mass fraction
14%, it embathes at 25 DEG C 27 minutes, is washed after filtering, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, and copper phthalein green grass or young crops sulfonate is that mass ratio is
1:The combination of 2 copper phthalein green grass or young crops polysulfonate and copper phthalein green grass or young crops disulfonate, the dosage of copper phthalein green grass or young crops sulfonate is substrate mass fraction
13%, filtering, washing, drying, make cationic layer surface coat monolayer pigment anion layer after being embathed at 30 DEG C 36 minutes；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of three layers of cladding nano thickness
Expect 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, including base material, four layers of cationic layer and four
Layer pigment anion layer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer and pigment are cloudy
Sheath alternately coats, and one layer of outermost is pigment anion layer, and base material is titanium nacreous for cat gold, 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 5 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 70 DEG C 40 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2, the PDDA that titanate coupling agent will be immersed through the processed base material of step 1 and mass fraction is 3.5%
Mixed solution in, dosage that the dosage of titanate coupling agent is 0.21%, PDDA of substrate mass fraction is substrate mass point
Several 10% embathes 22 minutes, filtration washing after taking-up at 27 DEG C, and substrate surface is made to coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 9% of substrate mass fraction, filtering, washing, drying after being embathed at 28 DEG C 44 minutes make cationic layer surface cladding single
Layer pigment anion layer；
Step 4 is immersed in the solution for the PDDA that mass fraction is 3.5%, and the dosage of PDDA is substrate mass fraction
10%, it embathes at 27 DEG C 22 minutes, is washed after filtering, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 9% of substrate mass fraction, filtering, washing, drying after being embathed at 28 DEG C 44 minutes make cationic layer surface cladding single
Layer pigment anion layer；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of four layers of cladding nano thickness
Expect 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, including base material, four layers of cationic layer and four
Layer pigment anion layer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer and pigment are cloudy
Sheath alternately coats, and one layer of outermost is pigment anion layer, and base material is titanium nacreous for cat gold, the material of cationic layer
Expect the combination for PAH and PDDA, the material of pigment cationic layer is the combination of copper phthalein green grass or young crops polysulfonate and 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 3 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 90 DEG C 24 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2 will be immersed through the processed base material of step 1 in the mixed solution of titanate coupling agent and salting liquid, titanium
The dosage of acid esters coupling agent is the 0.1% of substrate mass fraction, and salting liquid is that volume ratio is 1:2 mass fraction is 2.5%
Polyallylamine hydrochloride and the polydimethyl diallyl ammonium chloride that mass fraction is 3.5%, the dosage of salting liquid is base material
The 22% of mass fraction embathes 35 minutes, filtration washing after taking-up at 22 DEG C, and substrate surface is made to coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, and copper phthalein green grass or young crops sulfonate is that mass ratio is
1:The combination of 1 copper phthalein green grass or young crops polysulfonate layer and copper phthalein green grass or young crops disulfonate, the dosage of copper phthalein green grass or young crops sulfonate is substrate mass fraction
18%, filtering after 32 minutes, washing, drying are embathed at 25 DEG C, cationic layer surface is made to coat monolayer pigment anion
Layer；
Step 4 is immersed in salting liquid, and salting liquid is that volume ratio is 1:2 mass fraction is 2.5% polyallylamine
Hydrochloride and the polydimethyl diallyl ammonium chloride that mass fraction is 3.5%, the dosage of salting liquid is substrate mass fraction
22%, it embathes at 22 DEG C 35 minutes, is washed after filtering, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, and copper phthalein green grass or young crops sulfonate is that mass ratio is
1:The combination of 1 copper phthalein green grass or young crops polysulfonate layer and copper phthalein green grass or young crops disulfonate, the dosage of copper phthalein green grass or young crops sulfonate is substrate mass fraction
18%, filtering after 32 minutes, washing, drying are embathed at 25 DEG C, cationic layer surface is made to coat monolayer pigment anion
Layer；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of four layers of cladding nano thickness
Expect 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, including base material, five layers of cationic layer and five
Layer pigment anion layer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer and pigment are cloudy
Sheath alternately coats, and one layer of outermost is pigment anion layer, and base material is titanium nacreous for cat gold, 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 4 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 80 DEG C 30 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2, the PAH that titanate coupling agent will be immersed through the processed base material of step 1 and mass fraction is 2.5%,
The dosage of titanate coupling agent is that the dosage of 0.01%, PAH of substrate mass fraction is the 19% of substrate mass fraction, at 24 DEG C
Under embathe 32 minutes, washed after filtering, make substrate surface coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops disulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops disulfonate
For the 15% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 30 DEG C 47 minutes
Monolayer pigment anion layer；
Step 4 is immersed in the solution for the PAH that mass fraction is 2.5%, and the dosage of PAH is substrate mass fraction
19%, it is washed after filtering in 32 minutes is embathed at 24 DEG C, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops disulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops disulfonate
For the 15% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 30 DEG C 47 minutes
Monolayer pigment anion layer；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of five layers of cladding nano thickness
Expect 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, including base material, five layers of cationic layer and five
Layer pigment anion layer, base material are innermost layer, and substrate surface cladding first layer cationic layer, first layer cationic layer surface coats
First layer pigment anion layer, the first layer pigment anion layer cladding second layer cationic layer, then cationic layer and pigment are cloudy
Sheath alternately coats, and one layer of outermost is pigment anion layer, and base material is titanium nacreous for cat gold, 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：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 5 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 78 DEG C 22 minutes, solid obtained after filtering, spend from
Sub- water is dried after rinsing；
Step 2, the PDDA that titanate coupling agent will be immersed through the processed base material of step 1 and mass fraction is 3.5%
Mixed solution in, the dosage that the dosage of titanate coupling agent is 2.4%, PDDA of substrate mass fraction is substrate mass fraction
12%, embathed at 30 DEG C 30 minutes, filtration washing after taking-up, make substrate surface coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 10% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 25 DEG C 42 minutes
Monolayer pigment anion layer；
Step 4 is immersed in the solution for the PDDA that mass fraction is 3.5%, and the dosage of PDDA is substrate mass fraction
12%, it embathes at 30 DEG C 30 minutes, is washed after filtering, pigment anion layer surface is made to coat individual layer cationic layer；
Step 5 is immersed in the copper phthalein green grass or young crops polysulfonate solution that mass fraction is 8.0%, the dosage of copper phthalein green grass or young crops polysulfonate
For the 10% of substrate mass fraction, filtering, washing, drying, coat cationic layer surface after being embathed at 25 DEG C 42 minutes
Monolayer pigment anion layer；
Step 6, step 5 repeats afterwards Step 4: step 5 obtains the cationic layers and face of five layers of cladding nano thickness
Expect anion layer, one layer of outermost is pigment anion layer.
In short, the foregoing is merely presently preferred embodiments of the present invention, all equalizations made according to scope of the present invention patent
Variation and modification should all belong to the covering scope of patent of the present invention.
Claims (7)
1. a kind of mica titanium gold pigment with blue effect, it is characterised in that：Including base material, at least two layers of cationic layer and
At least two layer pigment anion layers, base material are innermost layer, and substrate surface coats first layer cationic layer, first layer 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 are titanium nacreous for cat gold；The material of cationic layer is polyallylamine hydrochloride, poly dimethyl two
The combination of one or both of allyl ammonium chloride；The material of pigment anion layer is copper phthalein green grass or young crops disulfonate, the blue or green more sulphurs of copper phthalein
The combination of one or both of hydrochlorate.
2. a kind of preparation method of the mica titanium gold pigment with blue effect, which is characterized in that comprise the following steps：
Volume ratio is 1 by step 1:The sulfuric acid that the hydrogen peroxide and mass fraction that 3~5 mass fraction is 30% are 98% mixes
It closes, obtains mixed solution；By base material immerse mixed solution in, embathed at 60~90 DEG C 20~40 minutes, spent after filtering from
Sub- water is dried after rinsing；
Step 2 will immerse in the mixed solution of titanate coupling agent and salting liquid through the processed base material of step 1,25~
It embathes at 30 DEG C 20~40 minutes, is washed after filtering, substrate surface is made to coat individual layer cationic layer；
Step 3 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, embathed at 25~30 DEG C 30~50 minutes
It filters, wash afterwards, drying, cationic layer surface is made to coat monolayer pigment anion layer；
Step 4 immerses in salting liquid, embathes at 25~30 DEG C 20~40 minutes, washed after filtering, make pigment anion layer
Surface coat individual layer cationic layer, salting liquid be mass fraction be 2.5% polyallylamine hydrochloride, mass fraction be
The combination of one or both of 3.5% polydimethyl diallyl ammonium chloride；
Step 5 is immersed in the copper phthalein green grass or young crops sulfonate solution that mass fraction is 8.0%, embathed at 25~30 DEG C 30~50 minutes
It filters, wash afterwards, drying, cationic layer surface is made to coat monolayer pigment anion layer.
3. a kind of preparation method of mica titanium gold pigment with blue effect according to claim 2, feature exist
In：It is repeated after step 5 Step 4: step 5 obtains the cationic layer of multilayer coating structure and pigment anion layer, one layer of outermost
For pigment anion layer.
4. a kind of preparation method of mica titanium gold pigment with blue effect according to claim 2, feature exist
In：Copper phthalein green grass or young crops sulfonate is the combination of one or both of copper phthalein green grass or young crops disulfonate, copper phthalein green grass or young crops polysulfonate.
5. a kind of preparation method of mica titanium gold pigment with blue effect according to claim 2, feature exist
In：The dosage of titanate coupling agent is the 0.01~0.6% of substrate mass fraction.
6. a kind of preparation method of mica titanium gold pigment with blue effect according to claim 2, feature exist
In：The dosage of salting liquid is the 6~25% of substrate mass fraction.
7. a kind of preparation method of mica titanium gold pigment with blue effect according to claim 2, feature exist
In：The dosage 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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Address after: 311501 No. 599, Baiyun East Road, Tonglu Economic Development Zone, Hangzhou, Zhejiang Patentee after: Hangzhou Huada Haitian Technology Co.,Ltd. Address before: 311501 No. 599, Baiyun East Road, Tonglu Economic Development Zone, Hangzhou, Zhejiang Patentee before: HANGZHOU HYDROTECH Co.,Ltd. |