CN102260421A - Magic-color nacreous aluminum powder pigment and preparation method thereof - Google Patents
Magic-color nacreous aluminum powder pigment and preparation method thereof Download PDFInfo
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- CN102260421A CN102260421A CN2011101519445A CN201110151944A CN102260421A CN 102260421 A CN102260421 A CN 102260421A CN 2011101519445 A CN2011101519445 A CN 2011101519445A CN 201110151944 A CN201110151944 A CN 201110151944A CN 102260421 A CN102260421 A CN 102260421A
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Abstract
The invention discloses a magic-color nacreous aluminum powder pigment and a preparation method thereof. The method comprises the following steps of: using aluminum powder with average particle size of 10-150 microns and with surface coated with a SiO2 film as a matrix raw material; by means of characteristics of inertness, acid resistance, heat resistance and transparency of the SiO2 film, depositing a nanometer titanium dioxide film on the transparent SiO2 film by using a chemical liquid phase deposition method under a condition with solution pH value of 1.5-2.5 and temperature of 60-80 DEG C; washing and drying the nanometer titanium dioxide film; and roasting a pigment under the protection of an inert gas for 0.5-1.0 h at 500-600 DEG C so as to obtain the high-gloss and magic-color nacreous aluminum powder pigment with a TiO2/SiO2/Al-based composite film. The pigment simultaneously obtains magic color interference effect of the nacreous pigment and excellent comprehensive properties of the metal aluminum powder pigment like electrical conductivity, high hiding power, shielding property, non-toxicity, environment friendliness and the like; and with a special decorative effect, the pigment can be widely used for high-end automobile finishes, high-end ornaments, surface finishes of high-end instruments, ink printing, toys for children and the like. The method disclosed by the invention has the advantages of simplicity, easiness and feasibility of industrialization.
Description
Technical field
The present invention relates to novel decorative chromatic metallic pigment technology field, particularly pearly-lustre illusion-colour aluminium powder pigment and preparation method thereof.
Background technology
Pearly-lustre illusion-colour aluminium powder pigment is to coat the nano titanium dioxide film that one deck has high refractive index at the flake aluminum substrate surface through siliconizing, a kind of novel inorganic non-metallic/metal composite---the aluminium base illusion-colour pearly pigment that the interference of utilizing light to produce on metal oxide film prepares.
This novel pigment has following characteristics:
(1) has the pearliness as the silks and satins or the metalluster and the effect of bright flicker.Metallic aluminium ductility is good, easily makes regular shape, size distribution is even, radius-thickness ratio is big flake aluminum, is good substrate raw material.Similar to the mica titanium nacreous material that with the flaky mica powder is substrate preparation, in the flake aluminum surface recombination behind the titanium dioxide layer of high refractive index, light produces multiple reflection, projection and refraction at membrane interface, can produce the intensive nacreous lustre.Control different TiO
2Membrane wrapping thickness, pigment can be multiple interference colors such as cash, red, purple, blue, green, can change the grey metal outward appearance of aluminium powder pigment dullness.Its high brightness, high chroma and significant flash of light combine, and can make by jewelry and produce gorgeous brilliant illusion-colour effect, and good decorate properties is arranged.
(2) the high opacifying power of tool, shielding is good.The flake aluminum smooth surface; intensive metalluster is arranged; have specular reflection light and good reflective thermal radiation ability; in coating, can form the successive metallic membrane; energy reflect visible light, ultraviolet ray and infrared rays make its heat-insulating property with reflective thermal radiation and supercoat not destroyed by ultraviolet ray, prolong the life-span of coating; the good provide protections of erosive such as shielding ambient atmos, moisture, light are specially adapted to high-grade automobile finish.
(3) fast light, weathering resistance is strong, thermotolerance, chemical resistant properties are good.Pearly-lustre illusion-colour aluminium powder pigment thermotolerance and unreactiveness that the surface has coated the inorganic, metal oxide film significantly improve, be difficult for oxidation, water-fast, anti-diluted acid, organic solvent-resistant and sulfuration, compare occasion and relative harsh conditions that common aluminium powder can be applicable to comparatively high temps, its adaptability is stronger, and use range is wider.
(4) have good conductive characteristic, can be used for some occasions if any particular requirements such as electroconductibility, thermal radiation reflectivity.
(5) good hydrophilic property, can be in water-borne coatings good distribution.
(6) have nontoxicity, can be used for food utensil, food product pack and toy for children.
In sum, pearly-lustre illusion-colour aluminium powder pigment is a kind of type material with good decorate properties and multiple property, and is of many uses.Yet it is very difficult to be with common aluminium powder that substrate coated titanium oxide compound prepares pearly-lustre illusion-colour aluminium powder pigment.Because titanium dioxide generally is to carry out in the hot acid liquid phase in on-chip deposition, and aluminium powder is very active, the utmost point is not acidproof, and the acid solution under the more not anti-heating state is difficult to adopt chemical liquid deposition to make aluminium base pearly-lustre illusion-colour pigment.Germany BASF AG adopts vapour deposition process in nineteen ninety, in fluidized-bed reactor aluminium powder is used the rare gas element fluidisation, feeds TiCl
4, reaction generates colourless TiO about 200 ℃
2Be deposited on the aluminium powder surface, make aluminium base pigment (US with rainbow tone
4978394)This method facility investment expense is big, long reaction time, and little in batches, the cost height is difficult to large-scale production; People such as Zhou Yi once utilized oxidizing reaction to generate the extremely thin and uniform oxide film of one deck on aluminium powder surface, make colorful aluminium powder at oxide film surface adsorption pigment dyestuff again and (see " aluminium powder chemical stain pre-test ", Zhou Yi, Jia Yangang, Yinshan Mountains academic periodical, the 2nd phase of nineteen ninety-five, P 30 ~ 33).Mainly by the colored substance colour developing, optical interference effects is not remarkable for its colored aluminium powder; People such as Wu Yin adopt organism coating method polymethylmethacrylate to be coated on the aluminium powder pigment that the aluminium powder surface obtains having golden flash effect under pH=9,70 ℃ (to see " preparation research of golden flash aluminum flake pigments ", Wu Yin, Li Fengsheng, Bai Huaping etc., the Materials Science and Engineering journal, 2006 the 6th phases, P923 ~ 925), but at the surface coated PMMA film of aluminium powder is not crystalline structure, the nacreous lustre DeGrain of product.
For this reason, the present invention adopts the flake aluminum of process siliconizing as the substrate raw material.This aluminium powder surface has coated the transparent SiO of one deck inertia
2Film both can keep the metalluster of aluminium powder pigment, can tolerate sour environment again.(see " Flake Aluminum Powder Coated SiO
2The research of film ", Ye Hongqi, Chen Jiana, Liu Hui etc., Shanghai coating, 2006 the 10th phases, p15 ~ 18).Utilize the SiO on aluminium powder surface
2Film has acidproof, heat-resisting, transparent characteristics, uses liquid phase deposition at SiO
2Coat one deck nano titanium dioxide film on the film again, with TiO
2/ SiO
2The preparation of/Al base complex method has the pearly-lustre illusion-colour aluminium powder pigment of high gloss.This method is simple, has industrialized feasibility.
Summary of the invention
The object of the present invention is to provide a kind of aluminium powder pigment and preparation method thereof with illusion-colour nacreous lustre.
Purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method with aluminium powder pigment of illusion-colour nacreous lustre is:
The first step adds the bag silicon chip shape aluminium powder of 4 ~ 10 parts of diameters at 10 ~ 150 μ m in massfraction in reaction vessel, add 50 ~ 100 parts water, fully stirs to form aluminium powder suspension.
The pH value of second step joint aluminium powder suspension is between 1.5 ~ 2.5, suspension slowly is warming up to 50 ℃ ~ 80 ℃, under stirring condition, in suspension, slowly add titanium salt solution, and drip sig water simultaneously to keep the pH value stabilization of suspension, make titanium salt solution can slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, treat that hydrated titanium dioxide deposits to after certain thickness reaches required interference color, stop to add titanium liquid and alkali lye, and stopped reaction behind continuation stirring 0.5 ~ 1.0h.
The 3rd step is extremely neutral with pigment filtering, washing, and is dry in about 110 ℃ ~ 120 ℃.
The 4th step placed calcining furnace with dried aluminium powder pigment, fed rare gas element, slowly was warming up to 500 ~ 600 ℃ by room temperature, promptly obtained aluminium base pearly-lustre illusion-colour pigment behind this roasting temperature 0.5 ~ 1.0h.
The preparation method of aluminium base illusion-colour pearly pigment provided by the present invention has following feature:
1, adopt the surface to coat SiO
2The aluminium powder of film is as the pigment substrate, and it is active to have solved the aluminium powder chemical property, and the problem that easily is corroded under acidic conditions makes follow-up titanium salt hydrolysis deposition to carry out smoothly.
2, adopt chemical liquid deposition, be coated with transparent SiO
2The aluminium powder surface deposition clad nano titanium dioxide of film is with TiO
2/ SiO
2The preparation of/Al base complex method has the pearly-lustre illusion-colour aluminium powder pigment of high gloss.This chemical liquid deposition is simple for process, and equipment is simple, and the titanium tetrachloride raw material is cheap and easy to get, is produced on a large scale.Different thickness by the control titanium dioxide coating can make the serial pearly-lustre illusion-colour aluminium powder pigment with different interference color.
3, be coated with hydration TiO
2Aluminium powder pigment need make hydrated titanium dioxide dehydration become TiO through calcining with pigment characteristics
2The outside surface epitaxial can produce the intensive optical interference effect.Aluminium powder is oxidation loss of gloss very easily at high temperature, and the present invention adopts protection of inert gas when calcining, guaranteed the high-luster of pearly-lustre illusion-colour aluminium powder pigment.
4, the prepared pearly-lustre illusion-colour of the present invention aluminium powder pigment have simultaneously pearly pigment bright-colored beauty, high refractive index, fast light weather-proof, chemical stability good and the distinctive strong metalluster of metallic aluminium powder pigment, conduction, high covering power, shielding and excellent comprehensive performances such as floatation characteristic, asepsis environment-protecting, can be widely used in the surface daub on a wall of high-grade automobile finish, high-grade ornament, top-grade instrument and ink printing, toy for children etc., optical property that it is unique and decorative effect can greatly promote by the value of decorations product.
Embodiment
Embodiment 1
Adding diameter in reaction vessel is the bag aluminum silicon powder pigment 10g of 10 ~ 60 μ m, adds 100g water, fully stirs to form aluminium powder suspension.The pH value of regulating suspension is 1.8 ± 0.3, and suspension slowly is warmed up to 60 ℃ ± 5 ℃, and under agitation condition, the speed with 1.0ml/min in suspension slowly adds TiCl
4Solution (TiCl
4Content is 50g/L), and drip the NaOH aqueous solution (NaOH content is 50g/L) simultaneously, to keep the pH value stabilization of suspension, make titanium salt slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, work as TiCl
4When solution added 70ml, pigment presented intensive silver color interference color, stops to add titanium liquid and alkali lye, stopped reaction behind the continuation stirring 30min.Pigment filtering, washing is to neutral, dry in about 110 ℃.Dried aluminium powder pigment is placed calcining furnace, feed nitrogen, slowly be warming up to 500 ℃ ± 20 ℃, promptly obtain silver-coloured lustre illusion-colour aluminium powder pigment at this roasting temperature 60min by room temperature.
Embodiment 2
Adding diameter in reaction vessel is the bag aluminum silicon powder pigment 5.0g of 10 ~ 60 μ m, adds 80g water, fully stirs to form aluminium powder suspension.The pH value of regulating suspension is being 2.2 ± 0.3, and suspension slowly is warmed up to 70 ℃ ± 5 ℃, and under agitation condition, the speed with 0.8ml/min in suspension slowly adds TiCl
4Solution (content is 50g/L), and drip the NaOH aqueous solution (content is 50g/L) simultaneously, to keep the pH value stabilization of suspension, make titanium salt solution slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, work as TiCl
4When solution added 60ml, pigment presented golden interference color, stops to add titanium liquid and alkali lye, stopped reaction behind the continuation stirring 30min.Pigment filtering, washing is to neutral, dry in about 120 ℃.Dried aluminium powder pigment is placed calcining furnace, feed nitrogen, slowly be warming up to 550 ℃ ± 20 ℃, promptly obtain golden pearly-lustre illusion-colour aluminium powder pigment at this roasting temperature 45min by room temperature.
Embodiment 3
Adding diameter in reaction vessel is the bag aluminum silicon powder pigment 10g of 10 ~ 150 μ m, adds 100g water, fully stirs to form aluminium powder suspension.The pH value of regulating suspension is being 2.0 ± 0.3, and suspension slowly is warmed up to 80 ℃ ± 5 ℃, and under agitation condition, the speed with 1.0ml/min in suspension slowly adds TiCl
4Solution (content is 50g/L), and drip the NaOH aqueous solution (content is 50g/L) simultaneously, to keep the pH value stabilization of suspension, make titanium salt solution slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, work as TiCl
4When solution added 75ml, pigment presented red interference color, stops to add titanium liquid and alkali lye, stopped reaction behind the continuation stirring 30min.Pigment filtering, washing is to neutral, dry in about 110 ℃.Dried aluminium powder pigment is placed calcining furnace, feed nitrogen, slowly be warming up to 600 ℃ ± 20 ℃, promptly obtain golden red pearly-lustre illusion-colour aluminium powder pigment at this roasting temperature 45min by room temperature.
Embodiment 4
Adding diameter in reaction vessel is the bag aluminum silicon powder pigment 10g of 10 ~ 40 μ m, adds 100g water, fully stirs to form aluminium powder suspension.The pH value of regulating suspension is being 2.0 ± 0.3, and suspension slowly is warmed up to 75 ℃ ± 5 ℃, and under agitation condition, the speed with 1.2ml/min in suspension slowly adds TiCl
4Solution (TiCl
4Content is 50g/L), and drip the NaOH aqueous solution (NaOH content is 50g/L) simultaneously, to keep the pH value stabilization of suspension, make titanium salt solution slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, work as TiCl
4When solution added 100ml, pigment presented intensive silver interference color, stops to add titanium liquid and alkali lye, stopped reaction behind the continuation stirring 40min.Pigment filtering, washing is to neutral, dry in about 110 ℃.Dried aluminium powder pigment is placed calcining furnace, feed nitrogen, slowly be warming up to 600 ℃ ± 20 ℃, promptly obtain silver-coloured lustre illusion-colour aluminium powder pigment at this roasting temperature 30min by room temperature.
Embodiment 5
Adding diameter in reaction vessel is the bag aluminum silicon powder pigment 10g of 10 ~ 100 μ m, adds 100g water, fully stirs to form aluminium powder suspension.The pH value of regulating suspension is being 1.8 ± 0.3, and suspension slowly is warmed up to 70 ℃ ± 5 ℃, and under agitation condition, the speed with 1.0ml/min in suspension slowly adds TiCl
4Solution (TiCl
4Content is 100g/L), and drip the NaOH aqueous solution (NaOH content is 50g/L) simultaneously, to keep the pH value stabilization of suspension, make titanium salt solution slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder surface, work as TiCl
4When solution added 80ml, pigment presented golden interference color, stops to add titanium liquid and alkali lye, stopped reaction behind the continuation stirring 50min.Pigment filtering, washing is to neutral, dry in about 120 ℃.Dried aluminium powder pigment is placed calcining furnace, feed argon gas, slowly be warming up to 500 ℃ ± 20 ℃, promptly obtain golden pearly-lustre illusion-colour aluminium powder pigment at this roasting temperature 60min by room temperature.
Claims (7)
1. pearly-lustre illusion-colour aluminium powder pigment is characterized in that this kind pigment is to coat one deck or alternately coat multilayer at the flake aluminum substrate surface to have the nano titanium oxide of high refractive index or other metal oxide film and make.
2. pearly-lustre illusion-colour aluminium powder pigment according to claim 1, the base material that it is characterized in that preparing pearly-lustre illusion-colour pigment are to adopt the surface to be coated with the flake aluminum with acid resistance of transparent silicon dioxide film.
3. pearly-lustre illusion-colour aluminium powder pigment according to claim 1, the mean particle size that it is characterized in that preparing the flake aluminum base material of pearly-lustre illusion-colour aluminium powder pigment is 10 μ m ~ 150 μ m.
4. the preparation method of the described pearly-lustre illusion-colour of claim 1 aluminium powder pigment, it is characterized in that the technical process that nano titanium dioxide film coats: the flake aluminum with acid resistance and the deionized water that the surface are coated with the transparent silicon dioxide film in container form 5 ~ 10% the suspended dispersed aqueous solution, regulator solution pH to 1.5 ~ 2.5 ± 0.3, heated solution to 60 ℃ ~ 80 ℃, slowly drip titanium salt solution, dripping alkali liquid is to keep the pH value of solution value stabilization simultaneously, make titanium salt slowly be hydrolyzed into hydrated titanium dioxide and uniform deposition on the aluminium powder substrate, promptly stop to feed in raw material when reaching setpoint color, keep identical temperature to continue stirring reaction 0.5 ~ 1.0h, with pigment filtering,, filter to neutral with the deionized water washing, dry down at 100 ~ 120 ℃.
5. above-mentioned dried pigment is put into stoving oven, under the protection of rare gas element pigment is being taken out behind 500 ℃ ~ 600 ℃ following roasting 0.5 ~ 1.0h, can obtain the described pearly-lustre illusion-colour of claim 1 aluminium powder pigment.
6. the preparation method of pearly-lustre illusion-colour aluminium powder pigment according to claim 4 is characterized in that the used titanium salt solution of deposition titanium oxide is formulated by titanium tetrachloride on the aluminium powder substrate.
7. the preparation method of pearly-lustre illusion-colour aluminium powder pigment according to claim 4, the rare gas element that feeds when it is characterized in that calcining is nitrogen or argon gas.
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Application publication date: 20111130 |