CN103819934A - Method for preparing coated rare earth sulfide pigment - Google Patents
Method for preparing coated rare earth sulfide pigment Download PDFInfo
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- CN103819934A CN103819934A CN201410073272.4A CN201410073272A CN103819934A CN 103819934 A CN103819934 A CN 103819934A CN 201410073272 A CN201410073272 A CN 201410073272A CN 103819934 A CN103819934 A CN 103819934A
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Abstract
The invention provides a method for preparing coated rare earth sulfide pigment, which comprises the following experimental steps: dispersing washed rare earth sulfide pigment in a mixed liquid of water, ethanol, ammonia water and tetraethoxysilane at room temperature; filtering the liquid after reaction for a certain time and collecting a filtrate for use; washing and drying the filtered matter, and obtaining the rare earth sulfide pigment with the surface uniformly coated with a layer of silicon dioxide. According to the preparing method provided by the invention, the experiment condition is mild, the filtrate generated during the experiment can be recycled and reused, the experimental process is environmentally friendly, and industrialization is facilitated. The coated rare earth sulfide pigment prepared through the method provided by the invention is completely coated, high in color degree, good in dispersancy and non-toxic and harmless, and has the advantages of improved thermostability and acid resistance; besides, active groups on the surface of the coated product facilitate follow-up modification of composite pigment, so that the application range of the rare earth sulfide is widened.
Description
Technical field
The present invention relates to a kind of preparation method of cladded type rare earth sulfide pigment, belong to the synthetic preparation field of inorganic green pigment.
Background technology
Increasingly serious along with China's environment situation, just all will be eliminated by a large amount of colored organic pigments that containing cadmium, chromium and the toxic heavy metals such as plumbous that use on market, and it is extremely urgent to find a kind of replacement product of environmental protection.From the beginning of the nineties in last century by France
(rhone-poulenc) company is successfully developed as the nontoxic colored organic pigments of novel rare-earth first, and Cubic rare earth sesquifide particularly lanthanum sulfide and cerium sulphide is subject to extensive pass as a kind of pigment of novel environment friendly.Rare earth sesquifide is in having the advantages such as brightness is high, good weatherability, and it is not too high having thermostability yet, the shortcoming that acid resistance is poor.
In order to improve the performance of rare-earth sulfide, on its surface, coated layer of substance is a kind of desirable method as protective layer.The preparation method that European patent EP 0203838 (A2) has just been described a kind of rare-earth sulfide mixture pigment has successfully been coated the oxide compound of layer of transparent on the surface of rare earth sulfide pigment, the thermostability of gained composite pigment and antacid having arrived significantly promote.
The object of the invention is to provide a kind of preparation method of cladded type rare earth sulfide pigment.The coating product that method therefor of the present invention obtains is complete, toxicological harmless, and dispersion force is good, and outstanding advantage is substantially not affect under the prerequisite of pigment color, and its thermostability and acid resistance are all improved.In addition, the surface active groups of the composite pigment obtaining by sol-gel method is conducive to the rear modification of composite pigment, makes the range of application of rare-earth sulfide more extensive.
Summary of the invention
The present invention relates to a kind of preparation method of cladded type rare earth sulfide pigment, experimental technique is: under room temperature, washed rare earth sulfide pigment is dispersed in the mixed solution of the water, ethanol, ammoniacal liquor and the tetraethoxy that prepare by a certain percentage; After reaction for some time, all substances in reaction vessel are filtered, the filtrate collection of gained is for subsequent use; By the filtrate washing of gained, dry, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Described rare earth sulfide pigment is lanthanum sulfide, cerium sulphide, praseodymium sulfide or neodymium sulfide.
Described washed rare-earth sulfide washing composition used is water and ethanol.
In described mixed solution, the ratio of water and ethanol is 1/10 to 1/1.
In described mixed solution the concentration of ammoniacal liquor be 1-100 milliliter/liter.
In described mixed solution the concentration of tetraethoxy be 1-20 milliliter/liter.
The described reaction times is 1-24 hour.
Filtrate being coated for rare earth sulfide pigment again that described collection is for subsequent use.
The experiment condition gentleness that preparation method of the present invention relates to, the recyclable recycling of solvent for use, experimentation environment-friendly and green, is easy to industrialization.The cladded type rare earth sulfide pigment that adopts the present invention to make is completely coated, and gorgeous degree is high, toxicological harmless, and dispersion force is good, and its thermostability and acid resistance are all improved.
Accompanying drawing explanation
Accompanying drawing 1 is the powder x-ray diffraction spectrogram of implementing 1 product, and X-coordinate is diffraction angle, and ordinate zou is diffracted intensity.
Accompanying drawing 2 is photos of implementing the transmission electron microscope of 1 product.
Embodiment
Embodiment 1
1g cerium sulphide pigment is respectively washed one time with distilled water and 95% ethanol; Be 1/4 by washed colo(u)rant dispersion at water and ethanol volume ratio, 25 milliliters/liter of ammonia concns, tetraethoxy concentration is in 200 milliliters of mixed solutions of 2.5 milliliters/liter; Room temperature reaction after 10 hours filters all substances in reaction vessel, and the filtrate collection of gained gets up; By the filtrate washing of gained, dry, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Change cerium sulphide into lanthanum sulfide, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 3
It is 1/6 that water and ethanol ratio are changed into, and other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 4
Change ammonia concn into 50 milliliters/liter, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 5
Change tetraethoxy concentration into 5 milliliters/liter, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 6
To change 24 hours the reaction times into, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 7
Change mixeding liquid volume into 500 milliliters, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Embodiment 8
Solvent used is changed into the filtrate of collection, other conditions, with example 1, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
Claims (8)
1. a preparation method for cladded type rare earth sulfide pigment, is characterized in that, experimental procedure is as follows: under room temperature, washed rare-earth sulfide is dispersed in the mixed solution of water, ethanol, ammoniacal liquor and tetraethoxy; After room temperature reaction for some time, the material in reaction vessel is filtered, filtrate collection is got up for subsequent use; By the filtrate washing obtaining and dry, obtain the evenly rare earth sulfide pigment of coated layer of silicon dioxide of appearance.
2. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, described rare earth sulfide pigment is lanthanum sulfide, cerium sulphide, praseodymium sulfide or neodymium sulfide.
3. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, described washed rare-earth sulfide washing composition used is water and ethanol.
4. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, in described mixed solution, the ratio of water and ethanol is 1/10-1/1.
5. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, in described mixed solution the concentration of ammoniacal liquor be 1-100 milliliter/liter.
6. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, in described mixed solution the concentration of tetraethoxy be 1-20 milliliter/liter.
7. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, the described reaction times is 1-24 hour.
8. according to the preparation method of a kind of cladded type rare earth sulfide pigment of claim 1, it is characterized in that, described collect filtrate for subsequent use can be again coated for rare earth sulfide pigment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410073272.4A CN103819934A (en) | 2014-02-25 | 2014-02-25 | Method for preparing coated rare earth sulfide pigment |
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| CN201410073272.4A CN103819934A (en) | 2014-02-25 | 2014-02-25 | Method for preparing coated rare earth sulfide pigment |
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| CN103819934A true CN103819934A (en) | 2014-05-28 |
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| CN201410073272.4A Pending CN103819934A (en) | 2014-02-25 | 2014-02-25 | Method for preparing coated rare earth sulfide pigment |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992660A (en) * | 2014-05-30 | 2014-08-20 | 景德镇陶瓷学院 | Red ZrO2-coated gamma-Ce2S3 pigment and preparation method thereof |
| CN104016717A (en) * | 2014-06-26 | 2014-09-03 | 景德镇陶瓷学院 | Preparation method of zirconium-silicate-coated cerium sulfide scarlet pigment and product prepared by same |
| CN104877392A (en) * | 2015-06-11 | 2015-09-02 | 景德镇陶瓷学院 | Preparation method of silica-coated cerium sulphide red pigment and prepared product thereof |
| CN108084736A (en) * | 2017-12-19 | 2018-05-29 | 中国科学院包头稀土研发中心 | A kind of technique of simple pollution-free processing rare earth sulfide pigment |
| CN109260037A (en) * | 2018-10-31 | 2019-01-25 | 中国科学院包头稀土研发中心 | A kind of multifunctional rare-earth colorant and preparation method thereof |
| CN109385117A (en) * | 2018-09-07 | 2019-02-26 | 中国科学院包头稀土研发中心 | A kind of environmentally protective rare-earth colorant and preparation method thereof for plastics |
| CN109651846A (en) * | 2017-12-28 | 2019-04-19 | 包头市宏博特科技有限责任公司 | A kind of post-processing approach of rare-earth sulfide |
Citations (6)
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|---|---|---|---|---|
| EP0203838A2 (en) * | 1985-04-30 | 1986-12-03 | Rhone-Poulenc Chimie | Use of coloured pigments based on rare earths sulphurs in plastics, paints, or vanishes |
| CN1201441A (en) * | 1995-09-18 | 1998-12-09 | 罗狄亚化学公司 | Rare-earth and alkali metal sulphide, method for preparing same and use thereof as pigment |
| CN1241987A (en) * | 1996-11-19 | 2000-01-19 | 罗狄亚化学公司 | Use of a beta rare earth sulphide as colouring pigment and method for preparing same |
| CN1426376A (en) * | 2000-03-30 | 2003-06-25 | 罗狄亚稀土公司 | Composition based on rare earth metal sulplide with improved chemical stability, its preparation method and use as pigment thereof |
| CN1621490A (en) * | 2003-11-28 | 2005-06-01 | 上海师范大学 | Process for preparing rare-earth red luminescent materials |
| CN101104746A (en) * | 2007-08-07 | 2008-01-16 | 中国科学院长春应用化学研究所 | Red rare-earth lanthanum cerium sulfide dye and preparation method thereof |
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2014
- 2014-02-25 CN CN201410073272.4A patent/CN103819934A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0203838A2 (en) * | 1985-04-30 | 1986-12-03 | Rhone-Poulenc Chimie | Use of coloured pigments based on rare earths sulphurs in plastics, paints, or vanishes |
| CN1201441A (en) * | 1995-09-18 | 1998-12-09 | 罗狄亚化学公司 | Rare-earth and alkali metal sulphide, method for preparing same and use thereof as pigment |
| CN1241987A (en) * | 1996-11-19 | 2000-01-19 | 罗狄亚化学公司 | Use of a beta rare earth sulphide as colouring pigment and method for preparing same |
| CN1426376A (en) * | 2000-03-30 | 2003-06-25 | 罗狄亚稀土公司 | Composition based on rare earth metal sulplide with improved chemical stability, its preparation method and use as pigment thereof |
| CN1621490A (en) * | 2003-11-28 | 2005-06-01 | 上海师范大学 | Process for preparing rare-earth red luminescent materials |
| CN101104746A (en) * | 2007-08-07 | 2008-01-16 | 中国科学院长春应用化学研究所 | Red rare-earth lanthanum cerium sulfide dye and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| CHEN GUANHONG等: "Preparation of SiO2 coated Ce2S3 red pigment with improved thermal stability", 《JOURNAL OF RARE EARTHS》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992660A (en) * | 2014-05-30 | 2014-08-20 | 景德镇陶瓷学院 | Red ZrO2-coated gamma-Ce2S3 pigment and preparation method thereof |
| CN103992660B (en) * | 2014-05-30 | 2015-11-18 | 景德镇陶瓷学院 | A kind of ZrO 2coated γ-Ce 2s 3the preparation method of red stain |
| CN104016717A (en) * | 2014-06-26 | 2014-09-03 | 景德镇陶瓷学院 | Preparation method of zirconium-silicate-coated cerium sulfide scarlet pigment and product prepared by same |
| CN104877392A (en) * | 2015-06-11 | 2015-09-02 | 景德镇陶瓷学院 | Preparation method of silica-coated cerium sulphide red pigment and prepared product thereof |
| CN104877392B (en) * | 2015-06-11 | 2017-12-08 | 景德镇陶瓷大学 | A kind of preparation method of silicon dioxide coating type red pigment cerium sulphide and its obtained product |
| CN108084736A (en) * | 2017-12-19 | 2018-05-29 | 中国科学院包头稀土研发中心 | A kind of technique of simple pollution-free processing rare earth sulfide pigment |
| CN108084736B (en) * | 2017-12-19 | 2020-07-24 | 包头中科世纪科技有限责任公司 | Simple pollution-free process for treating rare earth sulfide pigment |
| CN109651846A (en) * | 2017-12-28 | 2019-04-19 | 包头市宏博特科技有限责任公司 | A kind of post-processing approach of rare-earth sulfide |
| CN109651846B (en) * | 2017-12-28 | 2021-01-05 | 包头市宏博特科技有限责任公司 | Post-treatment method of rare earth sulfide |
| CN109385117A (en) * | 2018-09-07 | 2019-02-26 | 中国科学院包头稀土研发中心 | A kind of environmentally protective rare-earth colorant and preparation method thereof for plastics |
| CN109260037A (en) * | 2018-10-31 | 2019-01-25 | 中国科学院包头稀土研发中心 | A kind of multifunctional rare-earth colorant and preparation method thereof |
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Application publication date: 20140528 |