CN100362057C - Multi-layer coated effect interference pigment and preparation method thereof - Google Patents
Multi-layer coated effect interference pigment and preparation method thereof Download PDFInfo
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- CN100362057C CN100362057C CNB2005101264987A CN200510126498A CN100362057C CN 100362057 C CN100362057 C CN 100362057C CN B2005101264987 A CNB2005101264987 A CN B2005101264987A CN 200510126498 A CN200510126498 A CN 200510126498A CN 100362057 C CN100362057 C CN 100362057C
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- refractive index
- metal oxide
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- interference pigment
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Abstract
The present invention relates to a multi-layer coated interference pigment changing colors along with angle change. The present invention is prepared by using partial substrates or metal oxide flaky objects of which the cores are removed as carriers and using compounds with low refractive indexes and metal oxides with high refractive indexes for alternative coating. The present invention has an obvious optical effect that colors change along with the change of view angles, and is used for the industries of automobile paint, cosmetic formulas, paint, printing ink, plastics, glass, etc.
Description
Technical field:
The present invention relates to a kind of pigment, relate in particular to effect interference pigment of a kind of multiple coating and preparation method thereof.
Background technology:
Metal oxide-coated reaches certain thickness with coating on flat substrates, when irradiate light arrives coatingsurface, part incident light wave is reflected, part light is transmitted to down layer of surface by coating, produces reflection of light and transmission again, will produce " interference " phenomenon of light like this.If represent the coating refractive index with n, d is a coat-thickness, and then nd is the optical thickness of coating.Some reflected light (λ=2/Nnd (N is a positive integer, and λ is the reflected light wavelength)) are weakened by interference effect, and other reflected light (λ=(4/ (2N-1)) nd) are enhanced.
When the metal oxide of high refractive index and the compound of low refractive index alternately are coated on the flat substrates, when wherein two-layer or multilayer had identical optical thickness, so catoptrical color can strengthen along with the increase of the number of plies.But also can be by suitable design and the thickness of selecting coat, also can be strong especially as the color change of visual angle function.The basis that Here it is prepares strong interference pigment and effect interference pigment.Wherein effect interference pigment with the viewing angle difference, can present the continuous variation of the color between two or more interference color.
United States Patent (USP) (US4434010) has at first proposed a kind of multiple coating coated interference pigment, is base material with the metal aluminium flake, alternately applies with low refractive index and two kinds of transparent materials of high refractive index to form.For example low refractive index materials is SiO
2With high refractive index material be TiO
2
It is base material that Japanese Patent (JP1992/93206) has proposed with sheet mica and sheet glass, applies opaque metal layer earlier, alternately applies SiO again
2And TiO
2Multiple coating pigment.
More than two kinds of pigment all have very high gloss and good hiding rare, but transparency is not high.
European patent (EP0753545) discloses a kind of effect interference pigment, and this is (as TiO at transparent high refractive index
2) on the substrate, apply at least one group of multilayered structure, comprise the colourless coating of refractive index≤1.8, the selectivity of the partially transparent of refractive index 〉=2.0 absorbs or the coating of non-selective absorption.This pigment has adopted chemical vapour deposition (Chemical Vapour Deposition) and physical vapor deposition method (Physical Vapour Deposition) coating processes, thus technical sophistication, cost costliness, and quality product poor reproducibility.
In recent years, it is base material that many tame patents (Japanese JP2000-517374, U.S. US6656259, US6284032, Chinese CN1470569 etc.) have proposed with nonmetal or metallic compound, adopt liquid-phase chemistry deposition technique, rely on high and low refractive index material alternate multiple coating processes to prepare the method that strengthens coated interference pigment and effect interference pigment.The common feature of these patented technologies is: the flat substrates of employing can be that low refractive index materials is (as mica, glass, SiO more and more widely
2, Al
2O
3Deng), also can be that high refractive index material is (as TiO
2, Fe
2O
3Deng).The pigment of this patent has not had early stage metal base pigment " firmly " property gloss, has presented effectively " softening " property gloss.
Summary of the invention:
The invention provides a kind of effect interference pigment of multiple coating, it is that the metal oxide flap that part substrate (core) is removed is a base material with a kind of novel flap, alternately applies the high refractive index coating of metal oxides of the low refractive index compound of refractive index＜1.8 and refractive index 〉=2.0 successively and constitutes.It is base material that the present invention has adopted a kind of novel flap, and by reasonably selecting coat-thickness, the optical effect that the color of realization multi-coated interference pigment varies by angle of view makes pigment have glossiness and hiding rare preferably.
The effect interference pigment of multiple coating of the present invention, the metal oxide flap that adopts a kind of part substrate (core) to be removed is base material (carrier), this metal oxide flap is derived out by metal oxide-coated silicate compound substrate pigment, and its pigment centre portions substrate (core) has been removed.This metal oxide flap has the comparison even curface, and size and thickness are also easy to control, so be a kind of well coated substrate (carrier) again.Main is because after centre portions core (silicate compound substrate, refractive index is about 1.6) further is removed, and then is replaced by air (refractive index is 1.0), like this, makes the height of metal oxide reflect advantage (TiO for example
2Refractive index is 2.6～2.7) can discharge more fully.
It is 10～100 μ m that the metal oxide flap that the present invention uses has median size, preferred 15～60 μ m.Flap has the thickness of 0.2～6.0 μ m.The burning species of described metal oxide flap is at least a in titanium dioxide, ferric oxide (III) and the stannic oxide.
Part substrate (core) is a silicate compound in the metal oxide flap that component part substrate (core) is removed, and comprises natural mica, synthetic mica and glass.
Be applicable to that low refractive index compound of the present invention is SiO
2, Al
2O
3, B
2O
3Or MgF
2Deng, in the coating structure of pigment of the present invention, the coat-thickness of low refractive index compound is 150～300nm, preferred 200～280nm. evidence, when the coat-thickness of low refractive index compound was 150nm, multi-coated interference pigment of the present invention just can obtain the optical effect of apparent in view changeable colors along with angle; When the coat-thickness of low refractive index compound 〉=200nm, the changeable colors along with angle optical effect of multi-coated interference pigment will seem stronger.
High refractive index metal oxide of the present invention is by oxide compounds such as titanium dioxide, ferric oxide (III), stannic oxide, zirconium white, chromic oxide, cobalt oxide, zinc oxide and one or more mixture or the mixture in them thereof.
In the pigment structure of the present invention, high refractive index coating of metal oxides thickness is 20-200nm, preferred 20-100nm.Evidence: this thickness than book just can obtain extremely significant effect.
In order to reach more intensive visual angle color effect, in the multi-coated interference pigment of the present invention, low, high refractive index coating can repeated multiple times alternately apply.But be subjected to economically and the total coating thickness influence, can alternately apply 1～3 time, the different refractive index coating applies 6 layers at most.
The preparation technology of multiple coating effect interference pigment of the present invention is divided into two stages:
The preparation that fs is removed the metal oxide flap of substrate (core) for part.
Subordinate phase applies for above-mentioned flap being carried out the wet chemistry depositing operation.
The metal oxide flap that the present invention partly removes substrate (core) is that the silicate compound substrate pigment with metal oxide-coated is raw material, the part substrate is removed in mixed acid solution extraction dissolving through hydrofluoric acid and two kinds of mineral acid compositions, the mineral acid that is adopted has sulfuric acid, nitric acid, hydrochloric acid and phosphoric acid, the mixed acid solution weight percent concentration is 20～50%, hydrofluoric acid and mineral acid weight ratio are 1: 5～1: 10, mixed acid solution and pigment ratio are 6: 1～10: 1, the extracting operation temperature is 50～80 ℃, and the extracting operation time is 8～12 hours.If service temperature raises, the extraction time can reduce.
Consider the soundness of metal oxide flap, be applied to metal oxide flap of the present invention, at least also have part substrate (core) to be retained in the flap, because the housing centre portions of pure metal oxides flap is hollow, this structure is more prone to fragility.
The metal oxide flap that the present invention adopts, the rate of removing of centre portions substrate (core) is 20～80% (weight), preferred 40～60%, because metal oxide thickness of flap difference, particle diameter difference, the content of the core of residual centre portions (substrate) in the metal oxide flap is bigger, to particle diameter is 10～60 μ m flaps speeches, is about 15.0～60.0%.
Test shows, after metal oxide flap part substrate (core) is removed, compares with original pigment (leaving whole cores), and its glossiness, hiding rare all increase substantially.
The present invention adopts the wet chemistry depositing operation to the multiple coating of metal oxide flap, its method is: the metal oxide flap that the part substrate is removed is suspended in the deionized water, temperature and the pH value of adjusting suspension (are generally 60～90 ℃, PH is 6～12), metering drips the corresponding water-soluble inorganic salts solution of low refractive index compound then, and dripping dilute hydrochloric acid simultaneously, to keep pH value constant.After dropwising, restir 0.5 hour, and then temperature and the pH value of adjusting suspension on demand (are generally 60～80 ℃, PH is 2～9), metering drips the corresponding water-soluble inorganic salts solution of high refractive index metal oxide again, drips sig water simultaneously, and it is constant to keep pH value.After dropwising, continue constant temperature again and stirred 0.5 hour.At last after filtration, the washing, the oven dry and the calcining (calcining temperature is generally 200～900 ℃), after sieving, promptly finish again.
Among the multi-coated interference pigment preparation technology of the present invention, the corresponding water-soluble inorganic salts solution of low refractive index oxide compound can be selected Na
2SiO
3, AlCl
3, Na
2B
4O
7, MgSO
4And NaF.
Among the multi-coated interference pigment preparation technology of the present invention, the corresponding inorganic salt solution of high refractive index metal oxide is chosen as hydrochloride, as TiCl
4, SnCl
4, FeCl
3, CoCl
2, ZnCl
2, CrCl
3And ZrOCl
2Deng.
The coated interference pigment of the above-mentioned multiple coating that obtains can also further carry out the back and apply and aftertreatment.It is painted for the multiple coating coated interference pigment is carried out that the back applies, and it can be mineral dye or pigment dyestuff that the back applies painted used tinting material, and wherein mineral dye comprises iron oxide black, carbon black, low price titanium oxide, iron orchid, cobalt aluminate and chromium hydroxide; Pigment dyestuff comprises phthalocyanine pigment, azo pigment, quinacridine ketone pigment etc.Aftertreatment is for the multiple coating coated interference pigment being carried out surface modification, to improve the stability of pigment to light, water and weather, improving pigment consistency, dispersiveness and dispersion stabilization in use.The hydrate of oxide compound or oxide compound can be applied during aftertreatment in surface of pigments, also organic coupling agent etc. can be applied.
Integrate and can draw, multiple coating pigment of the present invention has following characteristics:
1, adopted a kind of carrier of novel multiple coating coated interference pigment, i.e. the metal oxide flap that is removed of part substrate (core).Because the part core in the flap is removed, and replaced by the lower air of refractive index, so strengthened the difference of high and low refractive index coating refractive index, constantly made the changeable colors along with angle optical effect of pigment show different more, and improved the glossiness and the hiding rare of pigment.
2, selected a kind of thickness of high and low refractive index coating newly for use.High and low refractive index coat-thickness is compared with pigment changeable colors along with angle (for example JP2000-517374, CN1470569, US6656259 etc.) in the past and all is in the relative thin scope, has so just reduced the cost of pigment coated coating.
3, because the part core is removed, also because high and low refractive index coat-thickness descends, make the tap density of pigment that decline by a relatively large margin be arranged, so just improved the utilising efficiency of pigment unit mass, the anti-heavy performance during use in medium is also better.
Pigment of the present invention can be used for industries such as painting dressing automobiles lacquer, cosmetic formulations and coating, printing-ink, plastic and glass.
Following examples are used to further describe the present invention, but non-limiting the present invention.
Embodiment 1
With the 100g rutile TiO
2The slightly weak golden coated interference pigment of coated mica (particle diameter is 10～60 μ m,, TiO
2Content is 38%), join in the 700g mixed acid solution, this solution is made up of hydrofluoric acid, sulfuric acid and phosphoric acid, and total concn is 50%, and wherein, hydrofluoric acid: sulfuric acid: the weight ratio of phosphoric acid is 2: 10: 4.After stirring, be warming up to 60 ℃, stirring at low speed is 10 hours under constant temperature.Then pigment is separated, through clean and dry, just obtained the light golden interference color TiO of 67g again
2Flap.Former TiO
2In the coated interference pigment, about 50% mica core has been removed.
With the above-mentioned TiO that obtains of 20g
2Flap is suspended in the 600ml deionized water, stirring strongly under the material, be warming up to 85 ℃, then with sig water levelling suspension PH to 8.5, in suspension, drip at leisure again and contain the sodium silicate solution 310ml that SiO2 concentration is 58.5g/l, in suspension, drip 15% hydrochloric acid soln simultaneously, constant to keep the suspension pH value.After dropwising, continued stirred suspension again 30 minutes.In suspension, drip concentration then and be 9.5% FeCl
3Solution makes the suspension pH value drop to 3.5.Continue again to drip FeCl to suspension
3Solution drips dilute NaOH solution simultaneously, makes the suspension pH value keep 3.5 constant, FeCl
3The total add-on of solution is 215ml.After dripping, constant temperature stirred 30 minutes again.
After apply finishing, filter and take out pigment, fully clean through deionized water, and through 110 ℃ of oven dry and 600 ℃ of calcinings 30 minutes, sieve through 120 eye mesh screens again, just obtain required coated interference pigment.
Through card-coating, can observe the strong variations of color significantly with the visual angle, from the vertical angle of view to the horizontal view angle, color is changed to xanchromatic through red, orange red, orange, orange continuously by strong red-purple.
Embodiment 2 (comparative example 1)
With the 20g rutile TiO
2The slightly weak golden pigments, mica (particle diameter 10～60 μ m, the TiO that apply
2Content is 38%) be suspended in the 600ml deionized water, under strong mixing, be warming up to 85 ℃, with alkali lye PH is aligned to 8.5 then, will contain SiO
2Concentration is that the sodium silicate solution 310ml of 58.5g/l is added drop-wise in the suspension at leisure, and it is constant to keep pH value with 10% hydrochloric acid simultaneously.After adding, restir 30 minutes is then aligned the suspension pH value to 3.5, is 9.5% FeCl with concentration
3Drips of solution is added in the suspension, and it is constant to keep the suspension pH value with sig water simultaneously, FeCl
3The total add-on of solution is 215ml.After dripping, constant temperature stirred 30 minutes again.
After apply finishing, pigment is separated after filtration, and fully clean,,, and sieved, so just obtain the effect interference pigment of required preparation with 120 eye mesh screens after 600 ℃ of calcinings 30 minutes again through 110 ℃ of oven dry through deionized water.
Through card-coating, the changeable colors along with angle that also can obviously observe pigment changes, by the vertical angle of view to the horizontal view angle, its color by redness to orange-yellow continuous variation.
Compare test
With the pigment that obtains among embodiment 1 and the embodiment 2 (comparative example 1), part by weight by 1g pigment and 10gPU slurry (the butanone diluent of polyurethane(s)) is mixed with colorant, and press with quadrat method card-coating on the black paper card, (U.S. X-Rite company produces to adopt order side and spectrophotometric color measurement instrument then, MA68 II type) color index of two kinds of pigment of measurement, measurement result is shown in the following table:
| Sample | L* | c * | Hiding rare (range estimation) | Changeable colors along with angle changing conditions (order side) vertical angle of view → horizontal view angle |
| Embodiment 1 | 86.7 | 54.8 | Fine | Purplish red → red → orange red → orange → orange → Huang |
| Embodiment 2 | 79.2 | 41.6 | Good | Red → orange red → orange → orange |
| Remarks | 1. color index (L*, c *) data near vertical angle of view (sight line and reflection ray angle are 15 °) time.2. L* is a glossiness.3. c *Be saturation ratio. | |||
Show by measurement result, the present invention makes carrier with the metal oxide flap that part substrate (core) is removed, prepared multi-coated interference pigment, with the metal oxide pigment that all keeps with the mica core is that the prepared multi-coated interference pigment of carrier is compared, the changeable colors along with angle of pigment of the present invention changes more apparent different, glossiness (L* value), look full degree (c
*Value) all improve by a relatively large margin, hiding rare is also better.
Claims (10)
1. the effect interference pigment of a multiple coating, it is characterized in that: with the metal oxide flap that is removed part sheet silicate compound substrate or core is carrier, by the low refractive index compound S iO of refractive index＜1.8
2, Al
2O
3, B
2O
3Or MgF
2And the high refractive index metal oxide of refractive index 〉=2.0 alternately applies and constitutes, and wherein said flaky silicic acid salt compound is natural mica, synthetic mica or glass.
2. the effect interference pigment of multiple coating as claimed in claim 1, it is characterized in that: it is 10～100 μ m that the metal oxide flap that described part substrate or core are removed has median size, thickness is 0.2～6.0 μ m, and wherein the rate of removing of substrate or core is 20～80%.
3. the effect interference pigment of multiple coating as claimed in claim 2 is characterized in that: it is 40～60% that described part substrate or core remove rate.
4. the effect interference pigment of multiple coating as claimed in claim 1, it is characterized in that: the metal oxide in the described metal oxide flap is one or more in titanium dioxide, ferric oxide and the stannic oxide.
5. the effect interference pigment of multiple coating as claimed in claim 1 is characterized in that: described high refractive index metal oxide is one or more mixture or the mixture in titanium dioxide, ferric oxide, stannic oxide, zirconium white, chromic oxide, cobalt oxide, the zinc oxide.
6. the effect interference pigment of multiple coating as claimed in claim 1, it is characterized in that: the thickness of low refractive index compound coat is 150～300nm, the thickness of high refractive index coating of metal oxides is 20～200nm.
7. the effect interference pigment of multiple coating as claimed in claim 6, it is characterized in that: the thickness of low refractive index compound coat is 200～280nm, the thickness of high refractive index coating of metal oxides is 20～100nm.
8. the effect interference pigment of multiple coating as claimed in claim 1, it is characterized in that: low refractive index compound and high refractive index metal oxide alternately apply 1～3 time.
9. as the preparation method of the effect interference pigment of any described multiple coating of claim 1 to 8, it is characterized in that:
1) preparation of partly removing the metal oxide flap of substrate or core: the silicate compound substrate pigment with metal oxide-coated is raw material, the part substrate is removed in mixed acid solution extraction dissolving through hydrofluoric acid and two kinds of mineral acid compositions, the weight percent concentration of mixed acid solution is 20%～50%, hydrofluoric acid and mineral acid weight ratio are 1: 5～1: 10, the weight ratio of the silicate compound substrate pigment of mineral acid mixing solutions and metal oxide-coated is 6: 1～10: 1, temperature during extraction is 50～80 ℃, and the time is 8～12 hours;
2) the above-mentioned part metal oxide flap of removing substrate or core carries out the wet chemistry depositing operation and applies: the metal oxide flap of removing substrate or core that will part is suspended in the deionized water, the aqueous solution that adds low refractive index compound and the corresponding inorganic salt of high refractive index metal oxide successively, make low refractive index compound and high refractive index metal oxide alternating deposit on the surface of flap, the temperature when applying the low refractive index compound is 60～90 ℃, pH value 6～14; Temperature is 60～90 ℃, pH value 2～9 when applying the high refractive index metal oxide, apply finish after with the applicator filtering separation, clean, drying and calcining and sieving.
10. as the effect interference pigment of any described multiple coating of claim 1 to 8, be used for automobile finish, cosmetic formulations, coating, printing-ink, plastic and glass industry.
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|---|---|---|---|
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|---|---|---|---|
| CNB2005101264987A CN100362057C (en) | 2005-12-14 | 2005-12-14 | Multi-layer coated effect interference pigment and preparation method thereof |
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| CN100362057C true CN100362057C (en) | 2008-01-16 |
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Cited By (1)
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|---|---|---|---|---|
| WO2011103713A1 (en) * | 2010-02-24 | 2011-09-01 | 汕头市龙华珠光颜料有限公司 | New flip-flop interference pigments |
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