CN102675931B - Golden effect pigment and production technology thereof - Google Patents
Golden effect pigment and production technology thereof Download PDFInfo
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- CN102675931B CN102675931B CN 201210141108 CN201210141108A CN102675931B CN 102675931 B CN102675931 B CN 102675931B CN 201210141108 CN201210141108 CN 201210141108 CN 201210141108 A CN201210141108 A CN 201210141108A CN 102675931 B CN102675931 B CN 102675931B
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Abstract
The invention discloses a golden effect pigment and a production technology thereof. The pigment comprises an inner core and cladded metallic oxide, wherein the inner core is a tablet-shaped base material; the cladded metallic oxide comprises three layers, the first layer is a mixed layer of titanium dioxide and stannic oxide; the second layer is a mixed layer of iron trioxide and aluminium oxide; and the third layer is a mixed layer of titanium dioxide and stannic oxide. The production technology for the pigment comprises the following steps of: putting the tablet-shaped base material of the inner core into deionized water to prepare suspension of which the solid-liquid mass ratio is 1:(5-50); then, successively cladding the metallic oxide; after the three layers are cladded, stirring for 30min; washing and filtering; drying at the temperature of 100-200DEG C; and calcining at the temperature of 700-900DEG C to obtain a finished product. The pigment manufactured by the technology has the advantages of ultrastrong chroma, golden color and simple technology, is bright and gorgeous, is easy to control and is suitable for industrial production.
Description
Technical field
The present invention relates to the mineral dye field, be specially a kind of golden effect pigment and production technique thereof.
Background technology
So-called effect pigment, also be colour lustre pigments, mainly comprises two classes, i.e. pearly pigment and metallic effect pigments.Wherein the nonmetal pigment such as pearly pigment we be referred to as effect pigment.All these pigment all have little and thin plates, thereby show strong gloss effect with the orientation that is arranged in parallel in application system.
Golden pigment (bronze) in the past, great majority are the brass alloys that form with copper, zinc and aluminium etc., its preparation method is that alloy molten is atomized into to coarse meal, then put into ball mill wet-milling slabbing coarse meal, tempered elimination internal stress, through dry ball mill pulverizing, finally by crossing the selection by winnowing classification, glazed surface is processed and is formed again.This golden pigment complete processing complexity, and inflammable and explosive, acid and alkali-resistance not while simultaneously applying, the weathering resistance extreme difference, easily the oxidation loss of gloss is eclipsed.
Current effect pigment belongs to the novel pigment product, the characteristics such as the physics and chemistry type is stable, nontoxic, rich color that it has.At industry-by-industry, obtain applying more widely.The most influential Merck KGaA company applies for a patent in China both at home and abroad, and patent application publication number is CN1384858A, and this patent relates to a kind of golden yellow pearly pigment and Application and preparation thereof, and its processing requirement at least coats five layers of metal oxide.
With regard to current product, the ubiquity fullness of shade is not high, and the coating number of plies is various, and complex manufacturing is restive, causes existing effect pigment expensive, especially take golden effect pigment as on the high side, and is difficult to stably manufactured.
Summary of the invention
The present invention is just for above technical problem, provides that a kind of to solve existing golden effect pigment depth of shade poor, and complex manufacturing, is difficult to the stable problem of controlling, and is specially a kind of golden effect pigment and production technique thereof.
Concrete technical scheme of the present invention is as follows:
The golden effect pigment of a kind of tool, comprise kernel and coated metal oxide, kernel is the strip base material, the surface of strip base material is coated metal oxide successively, the thickness of strip base material is the 0.1-10 micron, particle diameter is the 1-1000 micron, and the strip base material is any one in natural mica, artificial mica synthesis, glass flake, aluminum oxide or borate.
Replace successively coated metal oxide at described strip substrate surface.Coat altogether three layers, each layer of structure is followed successively by:
The first layer, titanium dioxide and tindioxide mixolimnion;
The second layer, ferric oxide and aluminium sesquioxide mixolimnion;
The 3rd layer, titanium dioxide and tindioxide mixolimnion.
A kind of production technique of golden effect pigment comprises the following steps:
A) the strip base material of kernel is put in deionized water, making the solid-liquid mass ratio is 1:(5-50) suspension;
B) carry out successively coated metal oxide, the first layer, be adjusted to 1.6-2.5 with mineral acid by the pH value of the suspension in step a), then by TiCl
4solution and SnCl
4solution mixes, and slowly joins in the suspension of adjusting after pH value, and with mineral alkali, to adjust pH value be 3-4 and keep stable simultaneously, and the control temperature of reaction is 70-85 ℃, and always coating optical thickness control is 150-170nm;
C) second layer slowly adds FeCl in reacted material in step b)
3with AlCl
3mixing solutions, controlling pH value with alkali lye is 3-4, temperature of reaction is controlled at 80-95 ℃, always coating that optical thickness controls is 200-240nm;
D) the 3rd layer, with mineral acid, the pH value of the suspension in step a) is adjusted to 1.6-2.5, then by TiCl
4solution and SnCl
4solution mixes, and slowly joins in the suspension of adjusting after pH value, maintains the pH value stabilization at 1.6-2.5 and keeps stable with mineral alkali simultaneously, and controls temperature of reaction is 70-85 ℃, and always coating optical thickness control is 400-420nm;
E) after three layers of coating, stir 30min, through washing, filter, dry at the temperature of 100-200 ℃, then finished product after 700-900 ℃ of calcining.
Mineral alkali in step b) and step d) is NaOH solution or ammoniacal liquor, and mineral acid is hydrochloric acid.
TiCl described in step b) and step d)
4the concentration of solution is 10%-30%, SnCl
4the concentration of solution is 50%, TiCl
4solution and SnCl
4volume ratio be (30-150): 1.
FeCl in step c)
3the concentration of solution is 50-120g/L, AlCl
3the concentration of solution is 100-300g/L, FeCl
3solution and AlCl
3the volume ratio of solution is (60-100): 1.
Mention clad ratio in above-mentioned technique, its mica sheet that is defined as unit mass is made the per-cent that the required oxide compound of pigment accounts for overall pigment mass.
Positively effect of the present invention is embodied in:
(1), the depth of shade of pigment is superpower, has color and luster as gold, bright and new gorgeous.
(2), technique is simple, is easy to control, more common multilayer coating structure technique is more suitable in suitability for industrialized production.
(3), with immediate production technique in the market, compare, our technique only needs three layers of coating, and the coating raw material related to also only has four kinds.From production cost, operability, weigh like this, this technique has more great market economy and is worth.
The accompanying drawing explanation
Fig. 1 is product structure schematic diagram of the present invention
Wherein, 1---base material, 2---the 3rd layer of coated metal oxide of the first layer coated metal oxide, 3---second layer coated metal oxide, 4---.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is described in further detail, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
The synthetic mica small thin slices is put in deionized water, making the solid-liquid mass ratio is 1:(5-50) suspension, then carrying out successively following three layers of coated metal oxide coats: the first layer is adjusted to 1.6-2.5 with mineral acid by above-mentioned pH of suspension value, the TiCl that is 10%-30% by concentration
4the SnCl that solution and concentration are 50%
4solution fully mixes, and slowly joins in above-mentioned suspension TiCl
4solution and SnCl
4the volume ratio of solution is (30-150): 1.Keep stable by mineral alkali regulate process pH value simultaneously.Temperature of reaction is controlled at 70-85 ℃.Total optical thickness that coats is controlled as 150-170nm; The second layer adds FeCl in above-mentioned reaction system
3with AlCl
3mixing solutions, FeCl wherein
3strength of solution is 50-120g/L, AlCl
3strength of solution is 100-300g/L, FeCl
3with AlCl
3liquor capacity than for (60-100): 1, pH value of reaction system is controlled at 3-4, temperature of reaction is controlled at 80-95 ℃.Total optical thickness that coats is controlled as 200-240nm; The 3rd layer, with mineral acid, the pH value of the suspension in step a) is adjusted to 1.6-2.5, then by TiCl
4solution and SnCl
4solution mixes, and slowly joins in the suspension of adjusting after pH value, maintains the pH value stabilization at 1.6-2.5 and keeps stable with mineral alkali simultaneously, and controls temperature of reaction is 70-85 ℃, and always coating optical thickness control is 400-420nm;
After three layers of coating, stir 30min, through washing, filtration, dry at the temperature of 100-200 ℃, then finished product after 700-900 ℃ of calcining.
Embodiment 2:
The artificial mica synthesis powder 50g that to get thickness be 10 microns, be fed into it in deionized water, makes solid-liquid
Than being the suspension of 1:6, then start the first layer coated metal oxide, with hydrochloric acid, above-mentioned pH of suspension value is adjusted to 2.2, the TiCl that is 20% by concentration
4the SnCl that solution and concentration are 50%
4solution fully mixes, and volume ratio is 50:1, slowly joins in above-mentioned suspension.By NaOH solution regulate process pH value, keep being stabilized in 2.2 simultaneously.Temperature of reaction is controlled at 70 ℃.Optical thickness is controlled at 180nm.
The second layer adds the FeCl3 solution of 50g/L and the mixing solutions of 300g/L AlCl3 in above-mentioned reaction system, and volume ratio is 80:1, and pH value of reaction system is controlled at 3.3, and temperature of reaction is controlled at 90 ℃.Optical thickness is controlled at 250nm.
The 3rd layer, with hydrochloric acid, above-mentioned pH of suspension value is adjusted to 2.2, the SnCl4 solution that the TiCl4 solution that is 20% by concentration is 50% with concentration fully mixes, and volume ratio is 50:1, slowly joins in above-mentioned suspension.By NaOH solution regulate process pH value, keep being stabilized in 2.2 simultaneously.Temperature of reaction is controlled at 70 ℃, and overall optics gauge control is arrived to 400nm.
After trilamellar membrane coats, stir 30min, through washing, filter, after 120 ℃ of oven dry, 760 ℃ of calcinings finished product.The finished product depth of shade is superpower, has color and luster as gold, bright and new gorgeous.
Example 3,
Getting thickness is 10 microns, the compound mica 60g that particle diameter is 555 microns, and making the solid-liquid mass ratio is 1:
50 suspension.
The first layer, be adjusted to 2.0 with hydrochloric acid by above-mentioned pH of suspension value, the TiCl that is 16% by concentration
4the SnCl that solution and concentration are 50%
4solution fully mixes, and volume ratio is 100:1, slowly joins in above-mentioned suspension.By NaOH solution regulate process pH value, keep being stabilized in 2.0 simultaneously.Temperature of reaction is controlled at 75 ℃.Optical thickness is controlled at 150nm.
The second layer adds the FeCl3 solution of 50g/L and the mixing solutions of 300g/L AlCl3 in above-mentioned reaction system, and volume ratio is 100:1, and pH value of reaction system is controlled at 3.3, and temperature of reaction is controlled at 90 ℃.Optical thickness is controlled at 230nm.
The 3rd layer, with hydrochloric acid, above-mentioned pH of suspension value is adjusted to 2.0, the SnCl4 solution that the TiCl4 solution that is 16% by concentration is 50% with concentration fully mixes, and volume ratio is 100:1, slowly joins in above-mentioned suspension.By NaOH solution regulate process pH value, keep being stabilized in 2.0 simultaneously.Temperature of reaction is controlled at 70 ℃, and overall optics gauge control is arrived to 400nm.
After trilamellar membrane coats, stir 30min, through washing, filter, after 120 ℃ of oven dry, 760 ℃ of calcinings finished product.The finished product depth of shade is superpower, has color and luster as gold, bright and new gorgeous.
Claims (5)
1. a golden effect pigment, comprise kernel and coated metal oxide, it is characterized in that: kernel is the strip base material, and the surface of strip base material is coated metal oxide successively, and the thickness of strip base material is the 0.1-10 micron, and particle diameter is the 1-1000 micron,
Coated metal oxide has three layers, the mixolimnion that the first layer is titanium dioxide and tindioxide, and total coating optical thickness of the first layer is 150-170nm; The mixolimnion that the second layer is ferric oxide and aluminium sesquioxide, always coating optical thickness is 200-240nm; The 3rd layer is the mixolimnion of titanium dioxide and tindioxide, and the coating optical thickness is 400-420nm, and the strip base material is any one in natural mica, artificial mica synthesis, glass flake, aluminum oxide or borate.
2. the production technique of a golden effect pigment according to claim 1 is characterized in that comprising the following steps:
A, the strip base material of kernel is put in deionized water, made the suspension that the solid-liquid mass ratio is 1:5-50;
B, carry out coated metal oxide successively, the first layer, be adjusted to 1.6-2.5 with mineral acid by the pH value of the suspension in step a, then by TiCl
4solution and SnCl
4solution mixes, and slowly joins in the suspension of adjusting after pH value, and with mineral alkali, to adjust pH value be 3-4 and keep stable simultaneously, and the control temperature of reaction is 70-85 ℃, and always coating optical thickness control is 150-170nm;
C, the second layer slowly add FeCl in reacted material in step b
3with AlCl
3mixing solutions, controlling pH value with alkali lye is 3-4, temperature of reaction is controlled at 80-95 ℃, always coating that optical thickness controls is 200-240nm;
D, the 3rd layer, be adjusted to 1.6-2.5 with mineral acid by the pH value of the suspension in step c, then by TiCl
4solution and SnCl
4solution mixes, and slowly joins in the suspension of adjusting after pH value, maintains the pH value stabilization at 1.6-2.5 and keeps stable with mineral alkali simultaneously, and controls temperature of reaction is 70-85 ℃, and always coating optical thickness control is 400-420nm;
After e, three layers of coating, stir 30min, through washing, filter, dry at the temperature of 100-200 ℃, then finished product after 700-900 ℃ of calcining.
3. the production technique of golden effect pigment according to claim 2, it is characterized in that: the mineral alkali in step b and steps d is NaOH solution or ammoniacal liquor, mineral acid is hydrochloric acid.
4. the production technique of golden effect pigment according to claim 2, is characterized in that: the TiCl described in step b and steps d
4the concentration of solution is 10%-30%, SnCl
4the concentration of solution is 50%, TiCl
4solution and SnCl
4volume ratio be 30-150:1.
5. the production technique of golden effect pigment according to claim 2, is characterized in that: FeCl in step c
3the concentration of solution is 50-120g/L, AlCl
3the concentration of solution is 100-300g/L, FeCl
3solution and AlCl
3the volume ratio of solution is 60-100:1.
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|---|---|---|---|
| CN 201210141108 CN102675931B (en) | 2012-05-09 | 2012-05-09 | Golden effect pigment and production technology thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210141108 CN102675931B (en) | 2012-05-09 | 2012-05-09 | Golden effect pigment and production technology thereof |
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| CN102675931A CN102675931A (en) | 2012-09-19 |
| CN102675931B true CN102675931B (en) | 2013-12-25 |
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| CN104263017B (en) * | 2014-09-24 | 2016-01-27 | 南阳市凌宝珠光颜料有限公司 | A kind of preparation method of iron series crystal effect pigment |
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| US4814208A (en) * | 1986-10-09 | 1989-03-21 | Toyota Jidosha Kabushiki Kaisha | Finish coating method |
| JP2565716B2 (en) * | 1987-09-18 | 1996-12-18 | テイカ株式会社 | Titanium dioxide coated iron oxide pigment |
| JPH1075569A (en) * | 1996-08-29 | 1998-03-17 | Sanyo Electric Co Ltd | Active filter circuit |
| DE19746067A1 (en) * | 1997-10-17 | 1999-04-22 | Merck Patent Gmbh | Interference pigments based on flaky substrates used in paint, lacquer, printing ink, plastics, ceramics, glaze and cosmetics |
| CN1323117C (en) * | 2004-04-19 | 2007-06-27 | 付建生 | Pigment changed color as changing angle, and fabricating method |
| CN1266229C (en) * | 2004-08-10 | 2006-07-26 | 汕头市龙华珠光颜料有限公司 | Pigment of multi-gradition discolour at diffierent direction and production process thereof |
| EP1980594B1 (en) * | 2007-04-05 | 2009-06-03 | Eckart GmbH | Effect pigments comprising a glass flake substrate |
| CN101168624B (en) * | 2007-11-28 | 2012-02-15 | 四川大学 | Intelligent temperature-control functional mica nacreous pigment with multi-layer structure and preparation thereof |
| CN101200605A (en) * | 2007-12-10 | 2008-06-18 | 河北欧克精细化工股份有限公司 | Weather-resistant multiple-layer alteration paint and preparation method thereof |
| CN101235227A (en) * | 2008-03-13 | 2008-08-06 | 北京首创纳米科技有限公司 | Method for preparing mica titanium nacreous material |
| CN101353488A (en) * | 2008-09-25 | 2009-01-28 | 河北欧克精细化工股份有限公司 | High saturation degree multilayer nacreous pigment and preparation thereof |
| CN101353487A (en) * | 2008-09-25 | 2009-01-28 | 河北欧克精细化工股份有限公司 | Multi-layer multi-color changing colour change interval pigment and preparation thereof |
| CN101962492B (en) * | 2009-07-24 | 2014-01-08 | 林文广 | Novel multi-layer coating angularly heterochrome interference color pearlescent pigment |
| CN101974258A (en) * | 2010-10-14 | 2011-02-16 | 河北欧克精细化工股份有限公司 | Multilayer color change pigment with high saturation and preparation method thereof |
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Address after: 620866 Qinglong Avenue, economic development zone, Qinglong Town, Pengshan County, Meishan City, Sichuan Province Patentee after: Sichuan wanshengtong Precision Machinery Manufacturing Co.,Ltd. Address before: 620866 Qinglong Avenue, economic development zone, Qinglong Town, Pengshan County, Meishan City, Sichuan Province Patentee before: SICHUAN CHUANHONG FINE CHEMICAL Co.,Ltd. |
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