CN104151876A - Preparation method of synthetic twinkling golden pearlescent pigment - Google Patents
Preparation method of synthetic twinkling golden pearlescent pigment Download PDFInfo
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Abstract
The invention provides a preparation method of a synthetic twinkling golden pearlescent pigment. According to the method, a silicate monocrystal wafer is firstly crystallized by a normal-pressure high-temperature melt crystallization process, TiO2, Fe2O3 and other oxides are deposited on the monocrystal wafer, and the twinkling golden pearlescent pigment is crystallized at high temperature. The method comprises the following steps: proportionally and evenly mixing potassium carbonate, quartz sand, magnesite, alumina and potassium fluosilicate, adding into a melting furnace, melting by heating, cooling to crystallize, separating the monocrystal wafer, dispersing in water, and adding titanium tetrachloride, iron trichloride and other raw materials under the pH value of 1.5-5 to carry out hydrolytic deposition until the deposition amount of the Fe2O3 is 5-30% and the deposition amount of the TiO2 is 10-50%; and dehydrating and calcining to obtain the golden pearlescent pigment. The golden pearlescent pigment is directly prepared from the silicate and the like, thereby being beneficial to controlling the product quality and production cost and reducing the environmental pollution.
Description
Technical field
The invention belongs to pigment technology field, be specifically related to a kind of preparation method of glittering golden pearly pigment of synthetic.
Background technology
Study On Mica is to take natural mica thin slice as base material, with special producing technique, is coated continuously one deck or alternately coated multilayer TiO
2, Fe
2o
3deng high refractive index metal oxide and the micro mist forming, coating mostly is transition element oxide compound and silicoaluminate, carbon black and the organic toners such as titanium, iron, zinc, tin.This oxide membranous layer is much higher compared with the optical index of base material, and itself is transparent again, therefore reflection of light and transmission are produced and disturbed, its gloss of filming is just as soft as pearl and give three-dimensional space texture.Nacreous mica pigment is nontoxic, fast light, heat-resisting, stable chemical nature, possesses that chromatogram is wide, strong coloring force, luminous intensity and the optical property such as metallic appearance is strong, physical strength is high.The research of white mica based pearlescent pigments is at present comparatively ripe, and the research of phlogopite based pearlescent pigments needs deeply.
Within 1963, du pont company utilizes nonmetalliferous ore raw material to develop a kind of artificial pearl's delustering pigment---mica titanium nacreous material, its application is very extensive, and major applications is in fields such as sedan limousine decorative paint, military equipment camouflage, coating, plastics, leather, printing-ink, pottery, makeup.In coating, it is easily uniformly distributed, and can make coating have good weathering resistance and light stability also can keep flash effect; In paint, it can improve the visual appearance of paint, strengthens weathering resistance, on automobile and large-scale amusement toy, is all widely applied; For plastics, rubber, make it present metalluster, improve light stability, also can strengthen printing and printing and dyeing effect; In makeup, because it is nontoxic, non-stimulated to skin, the function of uv reflectance, skin makeup skin care, can be in lipstick, eye shadow, shampoo, nail varnish, hair jelly, protective skin cream etc.
Expansion along with nacreous mica pigment range of application, its performance has been proposed to requirements at the higher level, because its opacifying power, tint permanence, the transparency, stability and photostabilization have unsatisfactory part, in application, be subject to certain limitation, so improving its performance is the main direction of current pearly pigment research.
Summary of the invention
The invention provides a kind of preparation method of glittering golden pearly pigment of synthetic, solved in the past with TiO
2with Fe
2o
3the poor problem of golden pearly pigment nacreous lustre of preparing for raw material.
The technical scheme that the present invention takes: adopt constant-pressure and high-temperature fusion-crystallization method, crystallization goes out silicate single wafer, depositing Ti O on single-chip
2with Fe
2o
3, at high temperature, crystallize into glittering golden pearly pigment.First selecting salt of wormwood, quartz sand, magnesia, aluminum oxide, potassium silicofluoride, titanium tetrachloride, iron trichloride, tin tetrachloride is raw material, first salt of wormwood, quartz sand, magnesia, aluminum oxide, potassium silicofluoride are mixed by a certain percentage, add heating and melting in melting furnace, crystallisation by cooling after melting, isolates single-chip.Then according to size, single-chip is sieved, be distributed in water, between pH=1.5～5, add the raw materials such as titanium tetrachloride, the iron trichloride deposition that is hydrolyzed, make Fe
2o
3deposition between 5～30%, TiO
2deposition is between 10～50%; Dewater again, calcine and become glittering golden pearly pigment.
The present invention directly prepares golden pearly pigment by silicate etc., is conducive to control quality product, production cost, reduced environmental pollution, and product color is bright-coloured.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and following examples only, for explaining the present invention, do not form limiting the scope of the present invention.
Experimental drug required for the present invention is as follows: salt of wormwood, quartz sand, magnesia, aluminum oxide, potassium silicofluoride, titanium tetrachloride, iron trichloride, hydrochloric acid, sodium hydroxide, tin tetrachloride, aluminum chloride etc.
Specific experiment process is as follows:
1 first will
Weigh and mix in proportion, pour in melting furnace and be warmed up to after 1000-1700 ℃, natural cooling crystallization.
2 peel off the single crystal of advantages of good crystallization, grind or sieve out 100 grams of single-chips.
3 are distributed to 100 grams of single-chips in 1L water, are uniformly dispersed, and are warmed up to 60-70 ℃, adjust between pH1.5-2.0, add tin tetrachloride solution (SnO
20.5-2wt%), use liquid caustic soda constant pH, wherein tin tetrachloride solution can only comprise a kind of material of tin tetrachloride and also can further comprise aluminum chloride.
4 complete previous step after, pH is adjusted between 1.8-2.5, temperature is adjusted to and between 70-80 ℃, adds titanium tetrachloride solution (TiO
25-50wt%), wherein titanium tetrachloride solution can only comprise a kind of material of titanium tetrachloride and also can further comprise Cerium II Chloride, uses liquid caustic soda constant pH.
5 complete after previous step, and pH is adjusted between 2.5-3.5, and temperature is adjusted to and between 75-85 ℃, adds liquor ferri trichloridi (Fe
2o
3wt5-45%), wherein liquor ferri trichloridi can only comprise a kind of material of iron trichloride, also can further comprise the wherein mixture of a kind of material or both arbitrary proportions of titanium tetrachloride or zinc chloride, uses liquid caustic soda constant pH.
6 carry out suction filtration, oven dry by the product having deposited, and then it are obtained to product in 700 ℃-800 ℃ of calcinings.
Example below will be further described the present invention, but content of the present invention is not limited to this completely.
Example 1
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 17.8%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 2
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 68g, magnesia (purity 99%) 78g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 45g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 17.8%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 3
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 68g, magnesia (purity 99%) 78g, anhydrous alumina (purity 98%) 32g, potassium silicofluoride (purity 99.5%) 40g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, Fe
2o
3clad ratio is 17.8%, uses the liquid caustic soda constant pH to 3.5 of 1mol/L simultaneously, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 4
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 2g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4120mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 28%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 19%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 5
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 2.0, by the TiCl of 2mol/L
4120mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 2.0 of 1mol/L, TiO simultaneously
2clad ratio is 27%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
380mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 22%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 6
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 68g, magnesia (purity 99%) 78g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 45g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4120mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 26.6%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
385mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 23.6%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 7
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4the FeCl of 100mL and 3.5mol/L
3the mixture of 80mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, Fe simultaneously
2o
3clad ratio is 19.8%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 2.8, by the TiCl of 2mol/L
460mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 2.8 of 1mol/L, TiO simultaneously
2clad ratio is 35.7%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 8
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o and 1g AlCl
36H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the constant pH value to 1.8 of liquid caustic soda of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 17.8%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 9
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5gSnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4the FeCl of 100mL and 3.5mol/L
3the mixture of 80mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 21.5%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
330mL and 1mol/LZnCl
210mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3total clad ratio is 29.5%, ZnO
2clad ratio is 0.8% continue to stir 1h after adding material, filters, washing, dries, and puts in retort furnace and burns 800 ℃, finally makes glittering golden pearly pigment.
Example 10
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4the FeCl of 60mL and 3.5mol/L
3the mixture of 40mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L simultaneously.
6 are raised to 80 ℃ by temperature, and pH is adjusted to 8.0, and the nine water water glass 100mL of 100g/L are added in suspension with the speed of 1mL/min, use the hydrochloric acid constant pH to 8.0 of 0.5mol/L, SiO simultaneously
2clad ratio is 2%.
7 reduce the temperature to 76 ℃, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4the FeCl of 60mL and 3.5mol/L
3the mixture of 40mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2total clad ratio is 26.4%, Fe
2o
3total clad ratio is 22% to continue to stir 1h after adding material, filters, washing, dries, and puts in retort furnace and burns 800 ℃, finally makes glittering golden pearly pigment.
Example 11
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1380 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 65 ℃, regulate pH=1.5, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 76 ℃ by temperature, and pH is adjusted to 2.5, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 85 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 17.8%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Example 12
1 first mixes Anhydrous potassium carbonate (purity content 99.9%) 20g, quartz sand (purity 99%) 65g, magnesia (purity 99%) 73g, anhydrous alumina (purity 98%) 28g, potassium silicofluoride (purity 99.5%) 43g.
2 pour material in melting furnace into and are warmed up to after 1500 ℃, are incubated 16 hours, natural cooling crystallization 30 days.
3 xln is broken, mill, cross 325-600 order sizing screen.
4 are distributed to the xln 50g separating in 500mL water, stir, and are warmed up to 75 ℃, regulate pH=1.7, by 1.5g SnCl
45H
2o is diluted to 100mL, with the speed of 2mL/min, adds in suspension.
5 are raised to 80 ℃ by temperature, and pH is adjusted to 1.8, by the TiCl of 2mol/L
4150mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 1.8 of 1mol/L, TiO simultaneously
2clad ratio is 33%.
6 are raised to 80 ℃ by temperature, and pH is adjusted to 3.5, by the FeCl of 3.5mol/L
365mL adds in suspension with the speed of 1mL/min, uses the liquid caustic soda constant pH to 3.5 of 1mol/L, Fe simultaneously
2o
3clad ratio is 17.8%, adds the rear stirring 1h that continues of material, and filtration, washing, oven dry, put in retort furnace and burn 800 ℃, finally makes glittering golden pearly pigment.
Claims (2)
1. the preparation method of the glittering golden pearly pigment of a synthetic, the method comprises the steps: silicate single wafer to be placed in reactor, add deionized water, regulating solid-liquid mass volume ratio is (1:8)～(10:1), temperature is controlled between 50 ℃～90 ℃, pH is controlled between 1.5～5, stir, then carry out successively following 3 layers coated:
The first layer: temperature is controlled at 60～70 ℃ to the arbitrary proportion mixture that adds tin tetrachloride or tin tetrachloride and two kinds of materials of aluminum chloride in above-mentioned reaction solution, regulates pH value to maintain all the time 1.5～2.0 with liquid caustic soda simultaneously.
The second layer: temperature is controlled at 70～85 ℃ to the arbitrary proportion mixture that adds titanium tetrachloride or titanium tetrachloride and two kinds of materials of Cerium II Chloride in the first layer reaction solution, regulates pH value to maintain all the time 1.8～2.5 with liquid caustic soda simultaneously.
The 3rd layer: temperature is controlled at 75～85 ℃, in second layer reaction solution, add the arbitrary proportion mixture of iron trichloride or iron trichloride and two kinds of materials of titanium tetrachloride or the arbitrary proportion mixture of iron trichloride and two kinds of materials of zinc chloride, with liquid caustic soda, regulate pH value to maintain all the time 2.5～3.5 simultaneously.
Then the 3rd layer of suspension suction filtration, washing, oven dry, in 700 ℃～800 ℃ calcinings, obtain above-mentioned glittering golden pearly pigment.
2. the preparation method of the glittering golden pearly pigment of a kind of synthetic according to claim 1, is characterized in that, described the 3rd layer of suspension meets Fe
2o
3deposition 5～30%, TiO
2deposition 10～50%.
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| CN106280575A (en) * | 2016-07-21 | 2017-01-04 | 四川省川宏精细化工有限公司 | A kind of paint pearlescent pigment and preparation method thereof |
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| CN102127321A (en) * | 2010-12-14 | 2011-07-20 | 广东维诺珠光颜料有限公司 | Method for preparing gold pearlescent pigment with high hue and high brightness |
| CN103183972A (en) * | 2011-12-21 | 2013-07-03 | 默克专利股份有限公司 | Effect pigments |
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2014
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1654548A (en) * | 2004-02-09 | 2005-08-17 | 默克专利股份有限公司 | Light interfere pigment |
| CN101434759A (en) * | 2007-11-12 | 2009-05-20 | 温州大学 | Preparation of high glaze glass-based pearlescent pigment |
| CN101970581A (en) * | 2007-11-16 | 2011-02-09 | 巴斯夫欧洲公司 | Bright interference pigments |
| 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 |
| CN102127321A (en) * | 2010-12-14 | 2011-07-20 | 广东维诺珠光颜料有限公司 | Method for preparing gold pearlescent pigment with high hue and high brightness |
| CN103183972A (en) * | 2011-12-21 | 2013-07-03 | 默克专利股份有限公司 | Effect pigments |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280575A (en) * | 2016-07-21 | 2017-01-04 | 四川省川宏精细化工有限公司 | A kind of paint pearlescent pigment and preparation method thereof |
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| CN104151876B (en) | 2015-11-25 |
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