CN102492312B - High-saturation iron-series pigment and production method thereof - Google Patents
High-saturation iron-series pigment and production method thereof Download PDFInfo
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Abstract
The invention provides a high-saturation iron-series pigment and a production method thereof. The high-saturation iron-series pigment is characterized in that: mica is taken as a substrate, high-refractivity substances and low-refractivity substances are alternatively coated on the substrate, the low-refractivity substances include silicon dioxide, aluminum trioxide and diboron trioxide, and the high-refractivity substances include titanium dioxide, tin dioxide, ferric oxide, cobalt oxide, zirconium dioxide and dichromium trioxide. The production method of the pigment is mainly characterized in that: a soluble salt which corresponds to each of the substances is hydrolyzed and precipitated on the surface of the mica substrate at an appropriate pH value, and the precipitated soluble salt is calcined at the temperature of 450-750 DEG C, so that a coating substance is transformed into an oxide. Compared with a synthetic silicon dioxide substrate, the method has the advantages of higher convenience for drawing materials, low price and reduction in the production cost of the high-saturation iron-series pigment. A hydrolyzing coating process is easy to operate and control, the thickness of a coating layer can be controlled through the color phase change of the pigment, and a production process is simple.
Description
Technical field
The invention belongs to the mineral dye field, be specifically related to high saturation iron serial pigment and production method thereof.
Background technology
Due to the mankind, to beautiful yearning, develop different riotous with colour pigment and carry out beautify life, high saturation pigment has the brightness suitable with pigment dyestuff and vividness.The high saturation pigment of producing at present is mainly to take the silicon-dioxide of synthetic to be substrate, adopt wet chemical technology at its surface clad oxide skin, because the substrate thickness of synthetic only has 200～500nm, and require very high to the substrate surface slickness, cost is high, to the generation Ben Taigao that makes such high saturation pigment.
The pearly pigment that employing is made at mica surface coated metal oxide layer, because a part of incident light is repeatedly reflected and reflects, make gloss have the degree of depth, thereby form nacreous lustre.Utilize pearly pigment can produce the principle of pearl effect, making to adopt mica to do the pigment that substrate prepares high saturation becomes possibility.Mica is the mineral substance with laminate structure, the mica powder that processing obtains generally all in the form of sheets, although being easy between layers of mica peeled away, but the mica surface formed thus easily produces ladder and unfairness, for the preparation of common pearly pigment, be feasible, but the pigment that will reach high saturation have difficulties.
Summary of the invention
The objective of the invention is to solve prior art and do with mica the defect that substrate can only prepare common pearly pigment, a kind of high saturation iron serial pigment and production method thereof of cooing substrate of mica is provided.
The present invention realizes that the technical scheme of above-mentioned purpose is as follows:
A kind of high saturation iron serial pigment, adopt mica powder to make substrate, first at mica surface, coats the metal oxide that one deck has high refractive index, pave the ladder of mica surface, and then coat the oxide compound that one deck has low-refraction, finally coat again the metal oxide that one deck has high refractive index
Wherein said oxide compound with low-refraction be in silicon-dioxide, alchlor, boron trioxide any one or wherein any two or three mix to use;
Described metal oxide with high refractive index is to select specific refractory power higher than silicon-dioxide, alchlor, boron trioxide, and water-fast metal oxide;
And have at least one deck to be coated with ferric oxide in the coating layer that the metal oxide of high refractive index forms.
Further, described metal oxide with high refractive index is a kind of in titanium dioxide, tindioxide, ferric oxide, cobalt oxide, zirconium dioxide, chromium sesquioxide, or the mixture of any two kinds and above composition.
The production method of above-mentioned high saturation iron serial pigment is as follows:
(1) mica powder is added to the water, dispersed with stirring obtains suspension, reheats to 60～90 ℃;
(2) regulate the pH of suspension value to desired value, the aqueous solution that adds again the corresponding soluble salt of metal oxide with high refractive index under stirring, after adding, ageing, this step will maintain the stable of pH of suspension value, and this pH value will be suitable for making the soluble salt added hydrolysis to generate precipitation;
(3) the pH of suspension value of gained after step (2) ageing is adjusted to desired value, the aqueous solution that adds again the corresponding soluble salt of oxide compound with low-refraction under stirring, after adding, ageing, this step will maintain the stable of pH of suspension value, and this pH value will be suitable for making the soluble salt added hydrolysis to generate precipitation;
(4) the pH of suspension value of gained after step (3) ageing is adjusted to desired value, the aqueous solution that adds again the corresponding soluble salt of metal oxide with high refractive index under stirring, after adding, ageing, this step will maintain the stable of pH of suspension value, and this pH value will be suitable for making the soluble salt added hydrolysis to generate precipitation;
(5) by step (4) gained suspension filtered, filter residue after washing drying after 450～750 ℃ of calcinings, then pulverize and sieve, drying obtains evengranular product.
Further, the described corresponding soluble salt of metal oxide with high refractive index is TiCl
4, TiOCl
4, SnCl
4, SnCl
2, FeCl
3, FeCl
2, CoCl
2, ZrOCl
2, CrCl
3.
Further, the described corresponding soluble salt of oxide compound with low-refraction is water glass, aluminum chloride, sodium aluminate, borax.
Further, be adopt concentrated hydrochloric acid or strong caustic to regulate the pH value of suspension or maintain the stable of pH of suspension value.The concentration of described concentrated hydrochloric acid is 18 % by weight, and the concentration of strong caustic is 15 heavy %.
The high saturation iron serial pigment made by described production process has:
Mica/Fe
2O
3/ SiO
2/ Fe
2O
3
Mica/SnO
2/ Fe
2O
3/ SiO
2/ Fe
2O
3
Mica/Fe
2O
3/ SiO
2/ Fe
2O
3/ Co
2O
3.
Beneficial effect of the present invention: high saturation iron serial pigment of the present invention, owing to adopting mica to cook substrate, is compared with synthetic silicon dioxide substrates, and it draws materials more convenient, cheap, has reduced the production cost of high saturation pigment.Hydrolysis coating process easy handling is controlled, and because the raw material added normally has color, therefore can by the foxy of pigment, judge the degree that hydrolytic precipitation carries out, and production process is simple.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1 structure: mica/Fe
2O
3/ SiO
2/ Fe
2O
3Preparation
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 750 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2200 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes.
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 750 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes.
(5) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
Embodiment 2 structures: mica/Fe
2O
3/ SiO
2/ Fe
2O
3/ Co
2O
3Preparation
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 1.5, under then stirring, be metered into the 60g/l tin tetrachloride solution of 10 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 850 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(4) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes.
(5) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 850 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes.
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
Embodiment 3 structures: mica/Fe
2O
3/ SiO
2/ Fe
2O
3/ Co
2O
3Preparation
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 950 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes.
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 950 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes.
(5) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 6.5, under then stirring, be metered into the 100g/l cobaltrichloride solution of 50 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
The prepared high saturation iron of embodiment 1～3 serial pigment adopts multi-angle color difference meter (model: Ai Seli MA68B) characterize.Comparative sample adopts the common iron series product of Ou Ke
Claims (4)
1. high saturation iron serial pigment, it is characterized in that: described high saturation iron serial pigment is to adopt mica powder to make substrate, first at mica surface, coat the metal oxide that one deck has high refractive index, pave the ladder of mica surface, and then coating one deck has the oxide compound of low-refraction, finally coat again the metal oxide that one deck has high refractive index
Wherein said oxide compound with low-refraction be in silicon-dioxide, alchlor, boron trioxide any one or wherein any two or three mix to use;
Described metal oxide with high refractive index is to select specific refractory power higher than silicon-dioxide, alchlor, boron trioxide, and water-fast metal oxide;
And have at least one deck to be coated with ferric oxide in the coating layer that the metal oxide of high refractive index forms;
And obtain one of by the following method:
Method one,
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 750 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2200 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 750 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(5) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying;
Method two,
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 1.5, under then stirring, be metered into the 60g/l tin tetrachloride solution of 10 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 850 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(4) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(5) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 850 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying;
Method three,
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 950 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 950 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(5) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 6.5, under then stirring, be metered into the 100g/l cobaltrichloride solution of 50 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
2. produce the method for high saturation iron serial pigment claimed in claim 1, it is characterized in that, detailed process is as follows:
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 750 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2200 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 750 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(5) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
3. produce the method for high saturation iron serial pigment claimed in claim 1, it is characterized in that, detailed process is as follows:
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 1.5, under then stirring, be metered into the 60g/l tin tetrachloride solution of 10 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 850 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(4) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(5) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 850 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
4. produce the method for the saturated iron serial pigment of height claimed in claim 1, it is characterized in that, detailed process is as follows:
(1) first by 32 gram white mica powders, particle diameter is 10～40 microns, joins in the deionized water of 500 milliliters and forms suspension, and be stirred and heated to 75 ℃;
(2) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 3.5, under then stirring, be metered into the 80g/l liquor ferri trichloridi of 950 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(3) then with 15 % by weight sodium hydroxide solutions, the pH value of suspension is transferred to 9.5 again, under stirring, the 35g/l sodium silicate solution of 2500 milliliters is dropwise added, in this process, dropwise add 18 % by weight hydrochloric acid solns to keep pH of suspension stable, after adding, constant temperature 30 minutes;
(4) and then with the hydrochloric acid of 18 % by weight the pH value of suspension is adjusted to 3.5, the 80g/l liquor ferri trichloridi that adds again 950 milliliters under stirring, in adition process, is that 15 % by weight sodium hydroxide solutions keep the pH of suspension value stabilization by concentration, after reinforced, constant temperature 30 minutes;
(5) then with the hydrochloric acid of 18 % by weight, the pH value of suspension is adjusted to 6.5, under then stirring, be metered into the 100g/l cobaltrichloride solution of 50 milliliters, the 15 % by weight sodium hydroxide solutions that add by dropwise in this process keep the pH value stabilizations, after reinforced, and constant temperature 30 minutes;
(6) last suspension after filtration, washing, drying, the calcining insulation is 20 minutes under 600 ℃, then pulverizes 100 mesh sieves, drying.
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| CN110358327A (en) * | 2019-07-25 | 2019-10-22 | 汕头市镇发珠光颜料有限公司 | A kind of high-purity red pearl effect pigment and preparation method thereof |
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| CN104327552B (en) * | 2014-09-25 | 2016-08-24 | 广西七色珠光材料股份有限公司 | A kind of high temperature resistant pearlescent pigment and preparation method thereof |
| CN104893366B (en) * | 2015-06-18 | 2016-07-06 | 广西七色珠光材料股份有限公司 | A kind of magnetic pearlescent pigment with 3D effect and preparation method thereof |
| CN106867280A (en) * | 2015-12-12 | 2017-06-20 | 福建坤彩材料科技股份有限公司 | Iron system pearlescent pigment of high chroma high brightness based on synthetic mica and its production and use |
| CN105482509A (en) * | 2015-12-15 | 2016-04-13 | 常熟市环虹化工颜料厂 | Method for preparing mica compounded pearlescent pigment |
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