CN104403376A - Preparation method of cobalt blue pigment - Google Patents
Preparation method of cobalt blue pigment Download PDFInfo
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- CN104403376A CN104403376A CN201410786384.4A CN201410786384A CN104403376A CN 104403376 A CN104403376 A CN 104403376A CN 201410786384 A CN201410786384 A CN 201410786384A CN 104403376 A CN104403376 A CN 104403376A
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- cobalt blue
- blue dye
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- presoma
- tio
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Abstract
The invention discloses a preparation method of cobalt blue pigment. The preparation method comprises steps as follows: (1), preparing a cobalt blue pigment precursor; (2), preparing an infrared reflection cobalt blue pigment precursor; and (3), preparing the cobalt blue pigment. The preparation method of the cobalt blue pigment is simple and convenient to operate and easy to implement, by means of doping of TiO2, the reflectivity of the cobalt blue pigment in a near-infrared region is improved, and the surface temperature of a dyed material is reduced; and moreover, reflectivity to blue light as well as brightness of the cobalt blue pigment is improved through doping of Ba<2+>, and the prepared cobalt blue pigment has excellent blue light development performance, lower heat absorption rate, excellent overall performance and broad application prospect.
Description
Technical field
The present invention relates to pigment art, particularly relate to a kind of preparation method of cobalt blue dye.
Background technology
Cobalt blue is a kind of pigment with spinel type crystal structure, mainly consists of cobalt oxide (CoO) and aluminum oxide (A1
2o
3), or be called Leyden blue [CoAl
2o
4].Cobalt blue dye is used for the painted of fluor in picture tube, require that it should to be tried one's best height to blue light reflectance, and as far as possible low to the light reflectance beyond blue light, briliancy is uprised, require that its reflectivity in near-infrared region is high as much as possible, to reduce the surface temperature of picture tube simultaneously.But the cobalt blue that industry uses now is not containing the pure CoAl of other metal ion
2o
4, such cobalt blue is not well positioned to meet every technology of colour picture tube, mainly there is following problem: the illuminant colour of (1) cobalt blue and the illuminant colour of fluor inconsistent, make the briliancy of blue light create reduction to a certain degree; (2) increase the content of Co in cobalt blue dye, the reflectance reduction to blue light while obtaining the good pigment of tinting strength, briliancy declines.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of cobalt blue dye, can solve the problems referred to above that existing cobalt blue dye exists.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of cobalt blue dye, comprises the steps:
(1) cobalt blue dye presoma is prepared: by (the NH of certain mass proportioning
4)
2c
2o
4and CoSO
4be placed in heated and stirred reactor, after adding distilled water dissolving, heated and stirred reaction certain hour, obtains reaction mixture solution, and filtration after precipitation leaves standstill, washing obtain cobalt blue dye presoma;
(2) infrared external reflection cobalt blue dye presoma is prepared: by TiO
2be dissolved in distilled water, be mixed with the slurries that concentration is 0.025 ~ 0.25g/mL, stir and make TiO
2abundant dispersion, then all adds TiO by the cobalt blue dye presoma of preparation in step (1)
2in slurries, heated and stirred is reacted, and obtains TiO
2the infrared external reflection cobalt blue dye presoma of doping vario-property;
(3) cobalt blue dye is prepared: by the TiO of preparation in step (2)
2the infrared external reflection cobalt blue dye presoma of doping vario-property, after precipitation, filtration, washing, drying, then adds the BaSO of certain proportioning
4, Al (OH)
3, become particle diameter to be the mixed powder of 50 ~ 80 μm with ball mill grinding, then mixed powder be placed in temperature programming stove, in an inert atmosphere, be warming up to 1300 ~ 1500 DEG C with the rate program of 100 ~ 300/min, insulation reaction 3 ~ 5h, in naturally near room temperature, obtain described cobalt blue dye.
In a preferred embodiment of the present invention, described (NH
4)
2c
2o
4and CoSO
4quality proportioning be 1:1.
In a preferred embodiment of the present invention, the heated and stirred reaction conditions in described step (1) is: Heating temperature 55 ~ 60 DEG C, stir speed (S.S.) 300 ~ 500 turns/min, reaction times 30 ~ 45min.
In a preferred embodiment of the present invention, the heated and stirred reaction conditions in described step (2) is: Heating temperature 90 ~ 100 DEG C, stir speed (S.S.) 50 ~ 100 turns/min, reaction times 2 ~ 3h.
In a preferred embodiment of the present invention, in described step (3), described infrared external reflection cobalt blue dye presoma, BaSO
4with Al (OH)
3mixing quality than for 10:0.5:0.5.
The invention has the beneficial effects as follows: the preparation method of a kind of cobalt blue dye of the present invention, easy and simple to handle, easily realize, by doped Ti O
2, improve the reflectivity of cobalt blue dye in near-infrared region, reduce the surface temperature of pollutant material; By doping Ba
2+, improve cobalt blue dye to blue light reflectance and briliancy, the cobalt blue dye prepared by the present invention has excellent blue light color developing and lower heat absorption rate, and excellent combination property, has a extensive future.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
A preparation method for cobalt blue dye, comprises the steps:
Be (the NH of 1:1 by quality proportioning
4)
2c
2o
4and CoSO
4be placed in heated and stirred reactor, add distilled water dissolve after, be heated to 55 DEG C, with the rotating speed stirring reaction 45min of 300 turns/min, obtain reaction mixture solution, precipitation leave standstill after filter, washing obtain cobalt blue dye presoma;
By TiO
2be dissolved in distilled water, be mixed with the slurries that concentration is 0.025g/mL, stir and make TiO
2abundant dispersion, then all adds TiO by the cobalt blue dye presoma prepared in above-mentioned steps
2in slurries, be heated to 90 DEG C, with the rotating speed stirring reaction 3h of 50 turns/min, obtain TiO
2the infrared external reflection cobalt blue dye presoma of doping vario-property;
Get TiO prepared by 10 parts of above-mentioned steps
2the infrared external reflection cobalt blue dye presoma of doping vario-property, after precipitation, filtration, washing, drying, then adds the BaSO that mass parts is 0.5 part
4with Al (OH)
3, become particle diameter to be the mixed powder of 50 μm with ball mill grinding, then mixed powder be placed in temperature programming stove, under nitrogen gas environment, be warming up to 1300 DEG C with the rate program of 100/min, insulation reaction 5h, in naturally near room temperature, obtain described cobalt blue dye.
Embodiment 2
A preparation method for cobalt blue dye, comprises the steps:
Be (the NH of 1:1 by quality proportioning
4)
2c
2o
4and CoSO
4be placed in heated and stirred reactor, add distilled water dissolve after, be heated to 60 DEG C, with the rotating speed stirring reaction 30min of 500 turns/min, obtain reaction mixture solution, precipitation leave standstill after filter, washing obtain cobalt blue dye presoma;
By TiO
2be dissolved in distilled water, be mixed with the slurries that concentration is 0.25g/mL, stir and make TiO
2abundant dispersion, then all adds TiO by the cobalt blue dye presoma prepared in above-mentioned steps
2in slurries, be heated to 100 DEG C, with the rotating speed stirring reaction 2h of 100 turns/min, obtain TiO
2the infrared external reflection cobalt blue dye presoma of doping vario-property;
Get TiO prepared by 10 parts of steps
2the infrared external reflection cobalt blue dye presoma of doping vario-property, after precipitation, filtration, washing, drying, then adds the BaSO that mass parts is 0.5 part
4with Al (OH)
3, become particle diameter to be the mixed powder of 80 μm with ball mill grinding, then mixed powder be placed in temperature programming stove, under nitrogen gas environment, be warming up to 1500 DEG C with the rate program of 300/min, insulation reaction 3h, in naturally near room temperature, obtain described cobalt blue dye.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a preparation method for cobalt blue dye, is characterized in that, comprises the steps:
(1) cobalt blue dye presoma is prepared: by (the NH of certain mass proportioning
4)
2c
2o
4and CoSO
4be placed in heated and stirred reactor, after adding distilled water dissolving, heated and stirred reaction certain hour, obtains reaction mixture solution, and filtration after precipitation leaves standstill, washing obtain cobalt blue dye presoma;
(2) infrared external reflection cobalt blue dye presoma is prepared: by TiO
2be dissolved in distilled water, be mixed with the slurries that concentration is 0.025 ~ 0.25g/mL, stir and make TiO
2abundant dispersion, then all adds TiO by the cobalt blue dye presoma of preparation in step (1)
2in slurries, heated and stirred is reacted, and obtains TiO
2the infrared external reflection cobalt blue dye presoma of doping vario-property;
(3) cobalt blue dye is prepared: by the TiO of preparation in step (2)
2the infrared external reflection cobalt blue dye presoma of doping vario-property, after precipitation, filtration, washing, drying, then adds the BaSO of certain proportioning
4, Al (OH)
3, become particle diameter to be the mixed powder of 50 ~ 80 μm with ball mill grinding, then mixed powder be placed in temperature programming stove, in an inert atmosphere, be warming up to 1300 ~ 1500 DEG C with the rate program of 100 ~ 300/min, insulation reaction 3 ~ 5h, in naturally near room temperature, obtain described cobalt blue dye.
2. the preparation method of cobalt blue dye according to claim 1, is characterized in that, described (NH
4)
2c
2o
4and CoSO
4quality proportioning be 1:1.
3. the preparation method of cobalt blue dye according to claim 1, is characterized in that, the heated and stirred reaction conditions in described step (1) is: Heating temperature 55 ~ 60 DEG C, stir speed (S.S.) 300 ~ 500 turns/min, reaction times 30 ~ 45min.
4. the preparation method of cobalt blue dye according to claim 1, is characterized in that, the heated and stirred reaction conditions in described step (2) is: Heating temperature 90 ~ 100 DEG C, stir speed (S.S.) 50 ~ 100 turns/min, reaction times 2 ~ 3h.
5. the preparation method of cobalt blue dye according to claim 1, is characterized in that, in described step (3), and described infrared external reflection cobalt blue dye presoma, BaSO
4with Al (OH)
3mixing quality than for 10:0.5:0.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410786384.4A CN104403376A (en) | 2014-12-18 | 2014-12-18 | Preparation method of cobalt blue pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410786384.4A CN104403376A (en) | 2014-12-18 | 2014-12-18 | Preparation method of cobalt blue pigment |
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| Publication Number | Publication Date |
|---|---|
| CN104403376A true CN104403376A (en) | 2015-03-11 |
Family
ID=52641050
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876283A (en) * | 2015-05-12 | 2015-09-02 | 上海大学 | Preparation method of anti-counterfeiting cobalt blue pigment with infrared reflectance function and fluorescence emission function |
| CN106629867A (en) * | 2016-12-21 | 2017-05-10 | 中国科学院兰州化学物理研究所 | Method for preparing light-blue cobalt blue hybrid pigment from aluminum-rich non-metallic minerals |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613779A (en) * | 2004-11-12 | 2005-05-11 | 南京大学 | Preparation for nanometer cobalt compound |
| CN101117452A (en) * | 2007-07-27 | 2008-02-06 | 陕西科技大学 | Method for preparing ultra-fine cobalt blue pigment under low-temperature |
-
2014
- 2014-12-18 CN CN201410786384.4A patent/CN104403376A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613779A (en) * | 2004-11-12 | 2005-05-11 | 南京大学 | Preparation for nanometer cobalt compound |
| CN101117452A (en) * | 2007-07-27 | 2008-02-06 | 陕西科技大学 | Method for preparing ultra-fine cobalt blue pigment under low-temperature |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876283A (en) * | 2015-05-12 | 2015-09-02 | 上海大学 | Preparation method of anti-counterfeiting cobalt blue pigment with infrared reflectance function and fluorescence emission function |
| CN106629867A (en) * | 2016-12-21 | 2017-05-10 | 中国科学院兰州化学物理研究所 | Method for preparing light-blue cobalt blue hybrid pigment from aluminum-rich non-metallic minerals |
| CN106629867B (en) * | 2016-12-21 | 2018-08-14 | 中国科学院兰州化学物理研究所 | The method for preparing high sapphirine cobalt blue hybrid pigment using rich aluminium nonmetallic mineral |
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Application publication date: 20150311 |