CN103804961B - A kind of blue effect pigment and preparation method thereof, purposes - Google Patents
A kind of blue effect pigment and preparation method thereof, purposes Download PDFInfo
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- CN103804961B CN103804961B CN201410040504.6A CN201410040504A CN103804961B CN 103804961 B CN103804961 B CN 103804961B CN 201410040504 A CN201410040504 A CN 201410040504A CN 103804961 B CN103804961 B CN 103804961B
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Abstract
The invention provides a kind of blue effect pigment, be included in substrate surface coated composites layer, and the silicon dioxide layer of described composite layer outer cladding, this pigment outward appearance is cobalt blue, there is good dispersiveness and two-color effect, due to the silica spheres of be coated with silicon oxide at the outermost layer of pigment layer and certain particle diameter, can prevent pigment " bonding die " in the time of high-temperature calcination, ensure that particle exists with dispersity to greatest extent, be conducive to be easy to disperse and large as far as possible performance color effect in the time of application; Make pigment have cubic light dispersion effect in the time of application, the light of reflection is softer simultaneously, and this pigment has high-temperature stability and weatherability, can be widely used in pottery, plastics and coating.
Description
Technical field
The present invention relates to chemical field, particularly a kind of blue effect pigment and preparation method thereof, purposes.
Background technology
Effect pigment is had to good optical effect for decorating, the one, give goods pearlescent gloss,This phenomenon is to be produced by the multi-level arrangement of the translucent particle of pearlescent pigment stratiform, be light at pigment andDifferent interfaces between base material, and all boundary layers of effect pigment itself are to light multiple reflections, refraction alsoForm the result of the interference of light. The 2nd, make the intangible surprised effect of vision. Therefore, thisKind have the pigment of special effect to be usually used to beautify the optical effect of article, and be widely used in cosmetics,In plastic cement, coating, leather and pottery.
Traditional double-colored pigment is the surface colour at pearlescent pigment, normally organic pigment or inorganic oxideThing. Organic pigment can not be high temperature resistant, and inorganic oxide does not have blueness. Patent US3951679 retouchesStated a kind of pigment, it taking pearlescent pigment as basis, in this surface of pigments Prussian blue clad, shouldPigment shortcoming is Prussian bluely at 200-300 DEG C of temperature, will decompose.
The pearlescent pigment that patent US4968351 describes, it is that adsorption coloring agent is painted, precipitation is coated on paintedIn agent with strengthening colouring agent absorption. The shortcoming of this pigment is in the time contacting with organic solvent, tonerTo separate from pearlescent pigment, this by all or part of lose color.
Indigo plant-the green pigment being made up of matrix and surface layer that patent US5169442 describes, matrix comprises uses metalBe oxidized coated mica, and surface layer is by the compositions of mixtures of magnesia, calcium oxide, cobalt oxide and titanium dioxide,The main look of this pigment is not pure blue.
The existing multi-coated interference pigment taking blueness as mass-tone, its design feature is " substrate/high index of refractionColourless, the transparent metal oxide layer/cobalt aluminate of colourless, transparent metal oxide layer/grazing shot rate, containing cobalt glassThe skin of glass or cobalt oxide ", or " substrate/cobalt aluminate, containing cobalt glass or cobalt oxide layer/grazing shot rate colourless,Colourless, the transparent metal oxide layer of transparent metal oxide layer/substrate/high index of refraction ".
To so far, all these blue or equal non-refractories of blue double-colored pigment (more than 1000 DEG C),And can not be used in refractory ceramics goods.
Summary of the invention
The object of the invention is to provide a kind of existing good dispersiveness and two-color effect, and its outward appearance look is gorgeousCobalt blue, has corresponding interference pigment, has again high-temperature stability and weatherability, can be widely used in pottery,In plastics and coating.
The blue effect pigment of one of realizing the object of the invention, is included in substrate surface coated composites layer, withAnd the silicon dioxide layer of described composite layer outer cladding.
Wherein said composite layer is the composite layer of aluminium oxide and cobalt oxide.
On wherein said silicon dioxide layer, then deposit layer of silicon dioxide ball.
Wherein said silica spheres particle diameter is 30-100nm.
The mol ratio of wherein said aluminium oxide and cobalt oxide is 1:6-6:1.
The percentage by weight of the each component of wherein said blue effect pigment is:
Aluminium oxide and cobalt oxide compound 5-50%
Silica 1-20%
Silica spheres 0-5%
Base material surplus.
Described blue effect pigment, wherein said base material is pearlescent pigment.
Wherein said pearlescent pigment is using mica, synthetic mica, tabular alumina or sheet silica as baseThe pearlescent pigment of sheet.
Described blue effect pigment, wherein said base material is sheet synthetic mica, natural mica, sheet oxygenChange aluminium and flaky silicon dioxide are that the titanium of substrate, surperficial cladding titanium dioxide is interference pigment.
A method of preparing described blue effect pigment, comprises the following steps:
(1) base material is mixed with appropriate pure water, form still liquid and heat up;
(2) be under agitation metered into metal salt solution, make substrate surface coated composites layer;
(3) add sodium silicate solution;
(4) solution above-mentioned steps being formed filters, washs, dries, calcines.
Wherein further comprise and adjust the temperature of described still liquid and the step of pH value.
Wherein said metal salt solution is the mixed liquor of aluminum salt solution and cobalt salt solution.
The temperature of wherein said still liquid is 60-90 DEG C, and described pH value is 7-9.
Wherein said calcining heat is 500-1100 DEG C.
Described blue effect pigment, for ceramic glaze.
Beneficial effect of the present invention:
Pigment of the present invention has good dispersiveness and two-color effect, and its outward appearance look is gorgeous cobalt blue, andThere are corresponding interference colours. There is high-temperature stability and weatherability, can be widely used in pottery, plastics and paintingIn material.
The present invention is due to the silica spheres of be coated with silicon oxide at the outermost layer of pigment layer and certain particle diameter,They can prevent pigment " bonding die " in the time of high-temperature calcination on the one hand, and particle adheres to each other each other,Ensure that particle exists with dispersity to greatest extent, be conducive to be easy to disperse with large as far as possible in the time of applicationThe effect of performance color; Owing to there being the light scattering effect of silicon ball, pigment is had in the time of application vertical on the other handBody light scattering effect, i.e. diffuse effect, the light of reflection is softer.
Because pigment flakes surface is coated with silicon oxide ball, there is anti-settling effect again, make preparation glaze,The pasty materials such as coating have and anti-fall effect, are conducive to pigment and are evenly distributed in material.
In a preferred embodiment of the invention, adopt pearlescent pigment prepared by resistant to elevated temperatures substrate as substrateTime, its resistance to elevated temperatures can reach more than 1100 DEG C, and outward appearance blueness is more gorgeous and be specially adapted to potteryIn glaze. When interference colours are while being blue, blue interference colours with the blue superimposed more gorgeous effect that obtains of outward appearanceAnswer pigment.
Detailed description of the invention
For better explanation the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete belowGround is described.
Embodiment 1:
A kind of blue effect pigment, its preparation method is:
(1) take titanium nacreous the putting into of blue interference colours synthetic mica that 30 gram particle footpaths are 10-60 micronVolume is in 2 liters of reactors, adds 800 ml deionized water, stirs and makes it dispersed one-tenth suspension;
(2) this suspension heated in thermostat water bath and be stabilized in 75 DEG C, the watery hydrochloric acid with 16% willThe pH of this suspension is adjusted to 7.50;
(3) add according to nCo with measuring pump2+:nAl3+The CoCl that=1:4 configures2·6H2O (0.25M) andAlCl3·6H2239.1 milliliters of O (0.25M) mixed liquors carry out regulator solution with 15% sodium hydroxide solution simultaneouslyIt is constant in above-mentioned pH value that pH makes it, and after reinforced, constant temperature stirs 15 minutes;
(4) with 15% NaOH, pH of suspension value is adjusted to 8.5, stirs 15 minutes, make pH dimensionBe held within the scope of this;
(5) by 50 milliliters of sodium silicate solution (SiO2Content is 20 grams per liters) slowly add with measuring pump,In this process, regulate pH value to make it constant with 16% hydrochloric acid, when reinforced complete, maintain reaction temperatureConstant, then stir 30 minutes;
(6) suspension is after filtration, with deionized water washing, dry at 120 DEG C,
(7) at 850 DEG C, calcine 30 minutes, after discharging, naturally cool to room temperature, obtain outward appearance withThe pearlescent pigment of blue color phase.
The structure that obtains pigment is as follows: titanium nacreous as base material using blue interference colours synthetic mica, and base materialAfter the compound of surface-coated aluminum oxide and cobalt oxide, then coated silica layer. Described aluminium oxide and oxidationThe mol ratio of cobalt is 1:4.
Embodiment 2
A kind of blue effect pigment, its preparation method is:
(1) take the titanium nacreous input of yellow interference colours synthetic mica that 30 gram particle footpaths are 10-60 micronBe in 2 liters of reactors to volume, add 800 ml deionized water, stir and make it dispersed one-tenth suspension;
(2) this suspension heated in thermostat water bath and be stabilized in 75 DEG C, the watery hydrochloric acid with 16% willThe pH of this suspension is adjusted to 7.50;
(3) add according to nCo with measuring pump2+:nAl3+The CoCl that=1:3 configures2·6H2O (0.25M) andAlCl3·6H2O (0.25M) mixed liquor 1225mL carrys out the pH of regulator solution simultaneously with 15% sodium hydroxide solutionMake it constant in above-mentioned pH value, after reinforced, constant temperature stirs 15 minutes.
(4) with 15% NaOH, pH of suspension value is adjusted to 8.5, stirs and pH was maintained in 15 minutesWithin the scope of this.
(5) by 50 milliliters of sodium silicate solution (SiO2Content is 20 grams per liters) slowly add with measuring pump,In this process, regulate pH value to make it constant with 16% hydrochloric acid, when reinforced complete, maintain reaction temperatureConstant, then stir 30 minutes.
(6) suspension is after filtration, with deionized water washing, dry at 120 DEG C,
(7) at 850 DEG C, calcine 30 minutes, after discharging, naturally cool to room temperature, obtain outward appearance withNavy blue, interference colours are yellow pearlescent pigment.
Acquisition pigment structure is: titanium nacreous as base material using yellow interference colours synthetic mica, and substrate surface bagCover after the compound of aluminium oxide and cobalt oxide, then coated silica layer. Rubbing of described aluminium oxide and cobalt oxideYou are than being 1:3.
The above, be only preferably detailed description of the invention of the present invention, but not office of protection scope of the present inventionBe limited to this, any be familiar with those skilled in the art the present invention disclose technical scope in, can be easilyThe variation of expecting or replacement, within all should being encompassed in protection scope of the present invention. Therefore, protection of the present inventionScope should be as the criterion with the protection domain of claims.
Claims (12)
1. a blue effect pigment, is included in substrate surface coated composites layer, and described multipleThe silicon dioxide layer of compound layer outer cladding; Wherein said composite layer is the composite layer of aluminium oxide and cobalt oxide,The mol ratio of described aluminium oxide and cobalt oxide is 1:6-6:1; The weight of the each component of described blue effect pigmentPercentage is:
Aluminium oxide and cobalt oxide compound 5-50%
Silica 1-20%
Silica spheres 0-5%
Base material surplus.
2. blue effect pigment according to claim 1, on wherein said silicon dioxide layer, more heavyLong-pending layer of silicon dioxide ball.
3. blue effect pigment according to claim 2, wherein said silica spheres particle diameter is30-100nm。
4. according to the arbitrary described blue effect pigment of claim 1-3, wherein said base material is pearly-lustre faceMaterial.
5. blue effect pigment according to claim 4, wherein said pearlescent pigment is with mica, sheetAluminium oxide or sheet silica are as the pearlescent pigment of substrate.
6. according to the arbitrary described blue effect pigment of claim 1-3, wherein said base material is that sheet is closedOne-tenth mica, natural mica, tabular alumina and flaky silicon dioxide are substrate, surperficial cladding titanium dioxideTitanium is interference pigment.
7. prepare as arbitrary in claim 1-5 as described in the method for blue effect pigment, comprise the following steps:
(1) base material is mixed with appropriate pure water, form still liquid and heat up;
(2) be under agitation metered into metal salt solution, make substrate surface coated composites layer;
(3) add sodium silicate solution;
(4) solution above-mentioned steps being formed filters, washs, dries, calcines.
8. the preparation method of blue effect pigment according to claim 7, wherein further comprises tuneThe step of the temperature of whole described still liquid and pH value.
9. the preparation method of blue effect pigment according to claim 7, wherein said slaine is moltenLiquid is the mixed liquor of aluminum salt solution and cobalt salt solution.
10. the preparation method of blue effect pigment according to claim 8, the temperature of wherein said still liquidDegree is 60-90 DEG C, and described pH value is 7-9.
The preparation method of 11. blue effect pigments according to claim 7, wherein said calcining heatFor 500-1100 DEG C.
12. as the blue effect pigment of claim 1,2,3,5 as described in arbitrary, for ceramic glaze.
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| CN201410040504.6A CN103804961B (en) | 2014-01-27 | 2014-01-27 | A kind of blue effect pigment and preparation method thereof, purposes |
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| CN201410040504.6A CN103804961B (en) | 2014-01-27 | 2014-01-27 | A kind of blue effect pigment and preparation method thereof, purposes |
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| CN103804961A CN103804961A (en) | 2014-05-21 |
| CN103804961B true CN103804961B (en) | 2016-05-11 |
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| CN108084795A (en) * | 2017-12-26 | 2018-05-29 | 佛山市高明丰霖新型材料有限公司 | A kind of ceramic ink zaffre and preparation method thereof |
| CN113979781B (en) * | 2021-11-24 | 2022-12-02 | 江西宏瑞新材料有限公司 | Temperature-resistant pearlescent mica sheet and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1508195A (en) * | 2002-12-17 | 2004-06-30 | Ĭ��ר���ɷ�����˾ | Inorganic ball-shape absorbing pigment |
| EP2100853A2 (en) * | 2008-03-07 | 2009-09-16 | Toda Kogyo Corporation | Infrared reflecting blue pigment, infrared reflecting green pigment, paint and resin composition using the infrared reflecting blue pigment, and paint and resin composition using the infrared reflecting green pigment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1508195A (en) * | 2002-12-17 | 2004-06-30 | Ĭ��ר���ɷ�����˾ | Inorganic ball-shape absorbing pigment |
| EP2100853A2 (en) * | 2008-03-07 | 2009-09-16 | Toda Kogyo Corporation | Infrared reflecting blue pigment, infrared reflecting green pigment, paint and resin composition using the infrared reflecting blue pigment, and paint and resin composition using the infrared reflecting green pigment |
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Address after: Industrial Zone Jinping District 515021 Guangdong city of Shantou province Sheng Ye Road No. 15 Patentee after: Guangdong Longhua New Material Co., Ltd Address before: Industrial Zone Jinping District 515021 Guangdong city of Shantou province Sheng Ye Road No. 15 Patentee before: SHANTOU LONGHUA PEARL LUSTRE PIGMENTS Co.,Ltd. |
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