CN109608906A - A kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment and preparation method thereof - Google Patents

A kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment and preparation method thereof Download PDF

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CN109608906A
CN109608906A CN201910064978.7A CN201910064978A CN109608906A CN 109608906 A CN109608906 A CN 109608906A CN 201910064978 A CN201910064978 A CN 201910064978A CN 109608906 A CN109608906 A CN 109608906A
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ultra
bismuth vanadate
yellow pigment
molybdenum bismuth
vanadate yellow
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CN109608906B (en
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王竹梅
李月明
左建林
孙熠
沈宗洋
宋福生
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Jingdezhen Ceramic Institute
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0006Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black containing bismuth and vanadium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating

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Abstract

The invention discloses a kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment, by Al2O3Transparent shell wrapping layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted.In addition, also disclosing the preparation method of above-mentioned ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment.Ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present invention, by aluminum oxide as transparent package shell, Coated molybdenum bismuth vanadate yellow pigment, significantly improves the heat-resisting quantity and acid resistance of molybdenum vanadic-acid bismuth-yellow pigment, and can satisfy higher use demand.The present invention uses wet chemistry method ultra-fine molybdenum pucherite particle obtained under liquid-phase condition, aluminum oxide package is carried out before undried, calcining, avoid the reunion and agglomeration of powder pigment, granules of pigments partial size it is thin and uniformly, good dispersion, and without expensive equipment, simple process is easy to operate, facilitates promotion and application.

Description

A kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment and preparation method thereof
Technical field
The present invention relates to inorganic pigment technical field more particularly to a kind of coated molybdenum bismuth vanadate yellow pigment and its preparations Method.
Background technique
Cadmium yellow (CdS) and chrome yellow (PbCrO4、BaCrO4), have many advantages, such as bright-colored, strong covering power, cheap, is Instantly the Inorganic yellow pigment generally used on the market, and applicating history is long, use scope is wide.However, due to contained Cadmium, lead and chromium (VI) poisoning metal element can seriously endanger human health and pollute environment, therefore, develop novel environment-friendly type yellow Color pigment is not only imperative to replace, more significant.
Molybdenum pucherite (general formula BiVO4·nBi2MoO6, 0.2≤n≤2) and it is a kind of Advanced Inorganic that novel environment friendly is nontoxic Yellow uitramarine, tone can be regulated and controled by the size of n value, and when n value is gradually increased, tone is yellow by red phase Huang Xiang Lvxiang Transformation, as n=0.75, the pigment yellow PY184 that the BASF AG as to have appeared on the market registers on pigment index, it is by four directions The BiVO of crystal form4With the Bi of rhombic form2MoO6The Yellow organic dye of the bright green of composition, strong covering power.
Currently, the manufacturing method of molybdenum bismuth vanadate yellow pigment has calcination and precipitating-calcination method.Calcination is By corresponding oxide or the salt that corresponding oxide can be generated through thermal decomposition by composition ingredient, after solid-phase ball milling mixes, in height The lower calcining of temperature.Precipitating-calcination method is first to dissolve corresponding water-soluble each salt ingredient, under the conditions ofs corresponding temperature and pH etc. Them are made to generate oxides or hydroxide gel precipitating, then in about 600 DEG C of temperature after the precipitating of generation is washed, dried Lower calcining, ultimately forms the BiVO mutually adjoined4And Bi2MoO6Two-phase crystallization.Above two method finally must wet-milling, suction filtration To reach corresponding granularity, not only technique is cumbersome, but also gained granules of pigments granularity is still larger, it is difficult to meet higher using need It asks.
In addition, the above-mentioned pigment of the prior art is intolerant to strong acid, and when being calcined to 600 DEG C or more, pigment can make because of sintering It darkens, loses glassy yellow, thus cannot be used under strong acid environment, also may not apply to the more demanding neck of temperature tolerance Domain, such as engineering plastics, high-temperature coatings, glass ink, ceramic paint.It therefore, is the service performance for improving pigment, to molybdenum vanadic acid Bismuth yellow uitramarine carries out the hot spot that surface modification treatment has become research and development, and the method mainly used at present is in the pigment Surface deposit colorless inorganic matter protective film, such as zirconium silicate, phosphate and various oxides, but pigment granules and nothing in the prior art Machine protective film be only mutual mixing and absorption together, protective film is not fine and close enough, therefore the effect is unsatisfactory.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of ultra-fine alumina coated molybdenum bismuth vanadate yellows Color pigment, by aluminium oxide as transparent package shell, Coated molybdenum bismuth vanadate yellow pigment, to significantly improve molybdenum pucherite The heat-resisting quantity and acid resistance of yellow uitramarine, and meet higher use demand.Another object of the present invention is to provide above-mentioned The preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment, first by the way that ultra-fine molybdenum vanadic acid is made under liquid-phase condition Bismuth yellow uitramarine carries out aluminium oxide package then without drying and calcination immediately, to obtain molybdenum vanadium ultra-fine, that package is fine and close Sour bismuth yellow uitramarine.
The purpose of the present invention is achieved by the following technical programs:
A kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment provided by the invention, by Al2O3Transparent shell package Layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted.The ultra-fine alumina coated molybdenum pucherite Yellow uitramarine average particle size is 0.5~1.0 μm, wherein the Al2O3The average thickness of transparent shell wrapping layer be 50~ 300nm。
In above scheme, its red scale value of yellow uitramarine of the present invention a*≤- 3.0, yellow value degree b* >=70;In air atmosphere Under in 1150 DEG C calcining after still be in bright-coloured bright yellow, red scale value a*≤- 1.0, yellow value degree b* >=68;It is aoxidized in glaze It is still in bright-coloured bright yellow, red scale value a*≤0, yellow value degree b* >=60 after the lower 800 DEG C of calcinings of atmosphere.The yellow uitramarine warp Concentration is that the salt acid soak 0.5h of 2mol/L is non-discolouring, weight-loss ratio < 15wt%.
Another object of the present invention is achieved by the following technical programs:
The preparation method of above-mentioned ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment provided by the invention, including following step It is rapid:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by bismuth nitrate (Bi (NO3)3·5H2O it) is dissolved in nitric acid solution, after dispersing agent stirring and dissolving is added, obtains To A liquid;
Molybdenum source and vanadium source are dissolved in sodium hydroxide solution by (1-2), according to molar ratio Mo: V: Bi=2.50~2.80: 0.60~0.64: 1, obtain B liquid;
(1-3) at room temperature mixes the A liquid and B liquid, and adjusting solution system pH value is 6.0~6.5, is stirring mixing water It is reacted under the conditions of bath, is then filtered, washed, obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake;
(2)Al2O3Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
The ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in dehydrated alcohol by (2-1), and distilled water and dense nitre is added After acid stirring, aluminium-alcohol salt is added according to molar ratio Al: Bi=1~4: 1, persistently stirring carries out aging reaction under water bath condition, Yellow sol is obtained after reaction;
(2-2) described yellow sol obtains ultra-fine alumina coated molybdenum bismuth vanadate yellow after cooling through drying, calcining Pigment.
Preparation method of the present invention uses wet chemistry method that the ultra-fine molybdenum pucherite of glassy yellow is made under liquid-phase condition first (Bi0.82V0.45Mo0.55O4), then wrapped up using the hydrolysis of aluminium-alcohol salt on molybdenum pucherite surface without drying and calcination Fine and close aluminum oxide, significantly improves the heat-resisting quantity and acid resistance of pigment, to obtain ultra-fine, high temperature-resistant acid-resistant molybdenum Bismuth vanadate yellow pigment.
Further, dispersing agent described in preparation method of the present invention is polyvinylpyrrolidone, neopelex, ten Six alkyl trimethyl ammonium bromides, polyvinyl alcohol, polyethylene glycol-800, cetomacrogol 1000, dosage be bismuth nitrate 5~ 8wt%.The molybdenum source is ammonium molybdate [(NH4)6Mo7O24·4H2O], molybdic acid disodium (Na2MoO4·2H2O);The vanadium source is inclined Sodium vanadate (NaVO3), ammonium metavanadate (NH4VO3);The aluminium-alcohol salt is aluminium secondary butylate (3 (C4H9O) .Al), aluminium isopropoxide (C9H21AlO3)。
Further, in step (1-1), (1-2) described in preparation method of the present invention nitric acid and sodium hydroxide solution concentration For 1.5~2.5mol/L;Step (1-3) the water-bath condition are as follows: 60~80 DEG C of temperature, 1.5~2.0h of reaction time.Institute State dehydrated alcohol (C in step (2-1)2H6O dosage) is according to molar ratio O: Bi=100~150: 1;Distilled water (the H2O) Dosage be according to molar ratio O: Al=4~8: 1;Concentrated nitric acid (the HNO3) dosage be according to molar ratio N: Al=5~6: 1;The bath temperature of the aging reaction is 50~70 DEG C, and the reaction time is 1.0~6.0h.Dried strip in the step (2-2) Part are as follows: temperature is room temperature~60 DEG C, relative humidity 25~35%;The calcination temperature is 800~900 DEG C.
The invention has the following advantages:
(1) ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present invention, granularity is small, and average particle size is 0.5~1.0 μm, it can satisfy higher use demand;Its inclusion enclave aluminium oxide, while the corrosion of extraneous strong acid can be completely cut off, one side pole The earth reduces the volatilization of Bi element at high temperature in pigment, it is ensured that tetragonal phase molybdenum pucherite (Bi0.82V0.45Mo0.55O4) Crystal phase stablize, to greatly improve the high-temperature stability of pigment;On the other hand make pigment that can prevent colorant at high temperature Sintering discoloration.It therefore, can also be at 1150 DEG C while ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present invention resistance to strong acid After being calcined in high-temperature calcination and 800 DEG C of fritted glazes, still keeps bright-colored, be greatly expanded its application field.
(2) present invention use wet chemistry method ultra-fine molybdenum pucherite particle obtained under liquid-phase condition, it is undried, forge Aluminium oxide package is carried out before burning, and avoids powder pigment reunion as caused by drying, calcining;Simultaneously as aluminium oxide Package makes pigment not agglomerate after 800~900 DEG C of calcinings, and therefore, granules of pigments is very thin, and uniform particle sizes, good dispersion are not required to Nanoscale yellow uitramarine powder can be obtained through subsequent wet-milling, suction filtration and stoving process.
(3) for preparation method of the present invention without expensive equipment, simple process is easy to operate, and influence factor is easy to control, facilitates Promotion and application.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 be ultra-fine molybdenum bismuth vanadate yellow pigment filter cake made from one step of the embodiment of the present invention (1-3) after drying Transmission electron microscope (TEM) photo;
Fig. 2 is the transmission electron microscope of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one (TEM) photo;
Fig. 3 is the XRD spectrum of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one.
Specific embodiment
Embodiment one:
A kind of preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present embodiment, its step are as follows:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by 9.70g Bi (NO3)3·5H2O is dissolved in the nitric acid solution that 100mL concentration is 2.0mol/L, is added After polyethylene of dispersing agent pyrrolidones 0.60g stirring and dissolving, A liquid is obtained;
(1-2) is by 9.76g ammonium molybdate [(NH4)6Mo7O24·4H2O] and 1.48g sodium metavanadate (NaVO3) it is dissolved in 100mL Concentration is to obtain B liquid in the sodium hydroxide solution of 2.0mol/L;
(1-3) at room temperature mixes above-mentioned A liquid and B liquid, is 6.0 with sodium hydroxide solution regulation system pH value, is stirring It mixes and stirs under the conditions of bath temperature is 70 DEG C and reacts 2.0h, after filtering, washed once first with a large amount of distilled water, then with anhydrous second Alcohol washed once, and obtaining ultra-fine molybdenum bismuth vanadate yellow pigment filter cake, (detection after drying is as shown in Figure 1, its good dispersion, is Irregular blocky, partial size is 100~200nm);
(2)Al2O3Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
Above-mentioned ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in 120mL dehydrated alcohol by (2-1), and 4mL distillation is added 7.5mL aluminium secondary butylate is added after stirring 0.5h in water and 12mL concentrated nitric acid, and after stirring and dissolving, water-bath is warming up to lasting stirring 60 ± 2 DEG C of progress aging reaction 2h, obtain yellow sol;
(2-2) after drying, calcines above-mentioned yellow sol under 60 DEG C of temperature, 30% relative humidity at 800 DEG C, heats up Speed is 5 DEG C/min, soaking time 1h, obtains ultra-fine alumina coated molybdenum pucherite after cooling (Bi0.82V0.45Mo0.55O4) yellow uitramarine.
As shown in Fig. 2, ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one, by Al2O3 Transparent shell wrapping layer and the molybdenum bismuth vanadate yellow powder pigment particle being coated in it are constituted, and dispersibility is preferable, shape Irregularly, partial size is 0.5~1.0 μm, wherein Al2O3The average thickness of transparent shell wrapping layer is 50~300nm.
From figure 3, it can be seen that ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from the embodiment of the present invention one is Tetragonal phase Bi0.82V0.45Mo0.55O4(PDF 85-0631), the wrapping layer of pigment are γ-Al2O3(PDF10-0425)。
Embodiment two:
A kind of preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present embodiment, its step are as follows:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
(1-1) is by 7.30g Bi (NO3)3·5H2O is dissolved in the nitric acid solution that 100mL concentration is 1.5mol/L, is added After polyethylene of dispersing agent alcohol 0.45g stirring and dissolving, A liquid is obtained;
(1-2) is by 10.0g molybdic acid disodium (Na2MoO4·2H2) and 1.06g ammonium metavanadate (NH O4VO3) to be dissolved in 100mL dense Degree is to obtain B liquid in the sodium hydroxide solution of 1.5mol/L;
(1-3) at room temperature mixes above-mentioned A liquid and B liquid, is 6.5 with sodium hydroxide solution regulation system pH value, is stirring It mixes and stirs under the conditions of bath temperature is 70 DEG C and reacts 2.0h, after filtering, washed once first with a large amount of distilled water, then with anhydrous second Alcohol washed once, and obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake;
(2)Al2O3Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
Above-mentioned ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in 120mL dehydrated alcohol by (2-1), and 3mL distillation is added 5.5g aluminium isopropoxide is added after stirring 0.5h in water and 10mL concentrated nitric acid, and after stirring and dissolving, water-bath is warming up to 60 with lasting stirring ± 2 DEG C of progress aging reaction 3h, obtain yellow sol;
(2-2) after drying, calcines above-mentioned yellow sol under 50 DEG C of temperature, 25% relative humidity at 900 DEG C, heats up Speed is 5 DEG C/min, soaking time 1h, obtains ultra-fine alumina coated molybdenum pucherite after cooling (Bi0.82V0.45Mo0.55O4) yellow uitramarine.
Embodiment three:
A kind of preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present embodiment is different from embodiment one Place is:
Vanadium source is ammonium metavanadate (NH in step (1-2)4VO3), dosage 1.42g;
Bath temperature is 65 DEG C in step (1-3);
The dosage of concentrated nitric acid is 14mL in step (2-1), and the dosage of aluminium secondary butylate is 9.5mL.
Example IV:
A kind of preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present embodiment is different from embodiment one Place is:
Molybdenum source is molybdic acid disodium (Na in step (1-2)2MoO4·2H2O), dosage 13.38g;Vanadium source is ammonium metavanadate (NH4VO3), dosage 1.42g;
Dehydrated alcohol dosage is 80mL in step (2-1), and the dosage of concentrated nitric acid is 9mL, and the dosage of distilled water is 3mL, secondary The dosage of aluminium butoxide is 6.0mL, and calcination temperature is 900 DEG C.
Embodiment five:
A kind of preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment of the present embodiment is different from embodiment two Place is:
Bi (NO in step (1-1)3)3·5H2The dosage of O is 9.70g;
Molybdic acid disodium (Na in step (1-2)2MoO4·2H2O dosage) is 12.9g;Ammonium metavanadate (NH4VO3) dosage For 1.45g;
The dosage of concentrated nitric acid is 12mL in step (2-1), and the dosage of aluminium isopropoxide is 7.0g.
Performance test:
1, colorimetric parameter test: using Hangzhou Yan Te Science and Technology Ltd. production the full-automatic chromascope of YT-ACM402 into Row test: simulation D65 working flare illumination, using d/0 illuminating watches geometrical condition, diffusion bulb diameter is 150mm, tests bore dia For 30mm, test wavelength range is visible light (400~700nm), surveys the colorimetric parameter CIE-L*a*b* of its pigment, wherein L* generation For table by black (0) to white (100), a* indicates that, by green (-) to red (+), b* is indicated by blue (-) to yellow (+).
2, acid resistance is tested: accurately being weighed 0.1000g colorant and is placed in dry centrifuge tube, 10mL concentration, which is added, is Clear liquid is carefully toppled over discarding by the salt acid soak half an hour of 2mol/L, centrifugation, twice with alcohol centrifuge washing, drying weighing, meter Calculate acid etching vector (wt%)=(G0-G1)/G0× 100%, wherein G0、G1The respectively forward and backward pigment weight of salt acid soak.
3, temperature tolerance test:
(1) naked burning temperature tolerance test: colorant is placed in alumina crucible, is kept the temperature in air atmosphere in a certain temperature spot 1h is calcined, surveys its colorimetric parameter after cooling.
(2) temperature tolerance test in low temperature frit glaze:
Colorant powder 0.5g is taken, with 1.5g low temperature frit (Al2O3-B2O3-SiO2- ZnO system) powder and 4mL deionized water Ground and mixed is formed uniformly glaze slip, it is evenly applied on the biscuit of ceramics being burnt into, and is heated up after dry with 10 DEG C/min To 800 DEG C, 10min is kept the temperature, its colorimetric parameter is surveyed after furnace cooling.
Such as 1 institute of table of the colorimetric parameter of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from various embodiments of the present invention Show.
With the yellow uitramarine of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake after drying made from one step of embodiment (1-3) (the ultra-fine molybdenum bismuth vanadate yellow pigment not wrapped up) as a comparison case.Obtained by the comparative example and various embodiments of the present invention Yellow uitramarine acid resistance test value it is as shown in table 2, the results are shown in Table 3 for naked burning temperature tolerance test, in low temperature frit glaze Temperature tolerance test the results are shown in Table 4.
The colorimetric parameter of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment made from 1 various embodiments of the present invention of table
The acid resistance test value of 2 various embodiments of the present invention of table and comparative example
3 various embodiments of the present invention of table and the comparative example calcined colorimetric parameter in air atmosphere
4 various embodiments of the present invention of table and the comparative example calcined colorimetric parameter in low temperature frit

Claims (10)

1. a kind of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment, it is characterised in that: by Al2O3Transparent shell wrapping layer, with And the molybdenum bismuth vanadate yellow powder pigment particle being coated in it is constituted.
2. ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 1, it is characterised in that: the ultra-fine oxygen Changing aluminium coated molybdenum bismuth vanadate yellow pigment average particle size is 0.5~1.0 μm, wherein the Al2O3Transparent shell wrapping layer Average thickness is 50~300nm.
3. ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 1 or claim 2, it is characterised in that: the Huang Its red scale value of color pigment a*≤- 3.0, yellow value degree b* >=70;In air atmosphere still in bright-coloured bright after 1150 DEG C of calcinings Yellow, red scale value a*≤- 1.0, yellow value degree b* >=68;It still becomes clear in bright-coloured after 800 DEG C of calcinings under oxidizing atmosphere in glaze Yellow, red scale value a*≤0, yellow value degree b* >=60.
4. ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 1 or claim 2, it is characterised in that: the Huang Color pigment is non-discolouring through the salt acid soak 0.5h that concentration is 2mol/L, weight-loss ratio < 15wt%.
5. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment, feature described in one of claim 1-4 exist In the following steps are included:
(1) preparation of ultra-fine molybdenum bismuth vanadate yellow pigment filter cake
Bismuth nitrate is dissolved in nitric acid solution by (1-1), after dispersing agent stirring and dissolving is added, obtains A liquid;
Molybdenum source and vanadium source are dissolved in sodium hydroxide solution by (1-2), according to molar ratio Mo: V: Bi=2.50~2.80: 0.60 ~0.64: 1, obtain B liquid;
(1-3) at room temperature mixes the A liquid and B liquid, and adjusting solution system pH value is 6.0~6.5, in stirring and water-bath item It is reacted under part, is then filtered, washed, obtain ultra-fine molybdenum bismuth vanadate yellow pigment filter cake;
(2)Al2O3Wrap up the preparation of molybdenum bismuth vanadate yellow pigment
The ultra-fine molybdenum bismuth vanadate yellow pigment filter cake is distributed in dehydrated alcohol by (2-1), and distilled water is added and concentrated nitric acid stirs After mixing, aluminium-alcohol salt is added according to molar ratio Al: Bi=1~4: 1, persistently stirring carries out aging reaction, reaction under water bath condition After obtain yellow sol;
(2-2) described yellow sol obtains ultra-fine alumina coated molybdenum bismuth vanadate yellow face after cooling through drying, calcining Material.
6. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature exist In: the dispersing agent be polyvinylpyrrolidone, neopelex, cetyl trimethylammonium bromide, polyvinyl alcohol, Polyethylene glycol-800, cetomacrogol 1000, dosage are 5~8wt% of bismuth nitrate.
7. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature exist In: the molybdenum source is ammonium molybdate, molybdic acid disodium;The vanadium source is sodium metavanadate, ammonium metavanadate;The aluminium-alcohol salt is sec-butyl alcohol Aluminium, aluminium isopropoxide.
8. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature exist In: the concentration of nitric acid and sodium hydroxide solution is 1.5~2.5mol/L in the step (1-1), (1-2);The step (1-3) Water-bath condition are as follows: 60~80 DEG C of temperature, 1.5~2.0h of reaction time.
9. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature exist In: the dosage of dehydrated alcohol is according to molar ratio O: Bi=100~150: 1 in the step (2-1);The dosage of the distilled water For according to molar ratio O: Al=4~8: 1;The dosage of the concentrated nitric acid is according to molar ratio N: Al=5~6: 1;The aging is anti- The bath temperature answered is 50~70 DEG C, and the reaction time is 1.0~6.0h.
10. the preparation method of ultra-fine alumina coated molybdenum bismuth vanadate yellow pigment according to claim 5, feature exist In: drying condition in the step (2-2) are as follows: temperature is room temperature~60 DEG C, relative humidity 25~35%;The calcination temperature is 800~900 DEG C.
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CN108585041A (en) * 2018-04-17 2018-09-28 河钢股份有限公司承德分公司 A kind of preparation method of the bismuth vanadium pigments of doping molybdenum element

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