CN105838112A - Chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment and preparation method thereof - Google Patents
Chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment and preparation method thereof Download PDFInfo
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- CN105838112A CN105838112A CN201610176268.XA CN201610176268A CN105838112A CN 105838112 A CN105838112 A CN 105838112A CN 201610176268 A CN201610176268 A CN 201610176268A CN 105838112 A CN105838112 A CN 105838112A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
Abstract
The invention discloses a chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment and a preparation method thereof. The preparation method includes the following steps: (1) dissolving CrCl3 and CdCl2 in distilled water to obtain a chromium-cadmium mixed solution; 2) dissolving Na2S and Se powder in distilled water to obtain a NaSSe solution; (3) with stirring, slowly adding dropwisely the NaSSe solution to the chromium-cadmium mixed solution and performing a reaction for 1 h completely; (4) allowing the mixture to stand for 1 h, performing suction filtration, washing the product with water and anhydrous alcohol, drying the product at 60 DEG C and grinding the product to obtain a precursor of the pigment; (5) moving the precursor into a porcelain crucible, placing the porcelain crucible in a muffle furnace, increasing the temperature to 500-600 DEG C, and maintaining the temperature for 30-60 min; and (6) ball-milling the product to a proper fineness to prepare the chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment. In the invention, a color developing body is generated in the solution and the doping element chromium is introduced, so that agglomeration of the precursor and uniform distribution of the doping element are controlled effectively. The preparation method is simple, is low in sintering temperature and improves the temperature-resistant capability of the pigment effectively.
Description
Technical field
The present invention relates to a kind of Red pigment and preparation method thereof, mix chromium type heatproof cadmium sulfoselenide crimson pigment and preparation method thereof particularly to one.
Background technology
Cadmium sulfoselenide crimson pigment is referred to as " Chinese red ", and color development is pure and bright-coloured, is to be presently available for red stain the most gorgeous in ceramic decoration.But, cadmium sulfoselenide colorant the most easily aoxidizes, and produces and decomposes, thus it is the most eclipsed to cause color and luster to decline, and seriously limits its application at ceramic field.The method being typically with zircon crystal parcel cadmium sulfoselenide at present in industry, utilize the heat-resisting ability of Zirconium orthosilicate. to solve the defect that cadmium sulfoselenide temperature resistant capability is weak, but this type of Red pigment production process is complicated, encapsulation ratio is low, and cannot ensure that fineness still has preferable temperature resistant capability to nanoscale.
Summary of the invention
It is an object of the invention to provide a kind of concise in technology, generated time is short, synthesis temperature is low, and has the cadmium sulfoselenide crimson pigment of certain temperature resistant capability and industrialization development potentiality and preparation method thereof.
For reaching above-mentioned purpose, the technical solution used in the present invention is: 1) by Cr: Cd=(1 ~ 5): the mol ratio of 100 is by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；2) S: Se=(2.5 ~ 4.5) are pressed: the mol ratio of 100 is by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 500 ~ 600 DEG C, take out after being incubated 30 ~ 60 minutes；6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
The invention have the benefit that the present invention to pass through in the solution and generate developing body and be simultaneously introduced doped chemical Cr, effectively control the reunion of presoma and being uniformly distributed of doped chemical, concise in technology, sintering temperature is low, from 500 ~ 600 DEG C (bright sulfur cadmium selenides), colorant temperature resistant capability can be brought up to 750 ~ 850 DEG C (mixing chromium type cadmium sulfoselenide).
Detailed description of the invention
Technical scheme is further illustrated below by specific embodiment.
Embodiment 1
1) mol ratio of Cr: Cd=3.2: 100 is pressed by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；2) mol ratio of S: Se=3: 100 is pressed by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 560 DEG C, take out after being incubated 30 minutes；6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
Embodiment 2
1) mol ratio of Cr: Cd=3.5: 100 is pressed by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；2) mol ratio of S: Se=3: 100 is pressed by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 540 DEG C, take out after being incubated 45 minutes；6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
Embodiment 3
1) mol ratio of Cr: Cd=2: 100 is pressed by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；2) mol ratio of S: Se=3: 100 is pressed by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 540 DEG C, take out after being incubated 30 minutes；6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
Embodiment 4
1) mol ratio of Cr: Cd=3.5: 100 is pressed by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；2) mol ratio of S: Se=3.5: 100 is pressed by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 560 DEG C, take out after being incubated 60 minutes；6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
Claims (1)
1. mix chromium type heatproof cadmium sulfoselenide crimson pigment and preparation method thereof for one kind, it is characterised in that:
1) Cr: Cd=(1 ~ 5) is pressed: the mol ratio of 100 is by CrCl3And CdCl2It is dissolved in distilled water and is made into CdCl2Concentration is the chromium cadmium mixed solution of 0.30mol/L；
2) S: Se=(2.5 ~ 4.5) are pressed: the mol ratio of 100 is by Na2S and Se powder is dissolved in distilled water and is made into Na2S concentration is the NaSSe solution of 0.30 mol/L；
3) under stirring condition, 1: 1 NaSSe solution is slowly dropped in chromium cadmium mixed solution by volume, fully reaction 1 hour；
4) after standing 1 hour, sucking filtration, washing, washes of absolute alcohol, 60 DEG C of drying, grind, obtain colorant presoma；
5) presoma is proceeded to porcelain crucible, be placed in Muffle furnace, be warming up to 500 ~ 600 DEG C, take out after being incubated 30 ~ 60 minutes；
6) ball milling is to after suitable fineness, obtains mixing chromium type heatproof cadmium sulfoselenide crimson pigment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610176268.XA CN105838112A (en) | 2016-03-28 | 2016-03-28 | Chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment and preparation method thereof |
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| CN201610176268.XA CN105838112A (en) | 2016-03-28 | 2016-03-28 | Chromium-doped temperature-resistant cadmium sulfoselenide bright red pigment and preparation method thereof |
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| CN105838112A true CN105838112A (en) | 2016-08-10 |
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2482006A (en) * | 1946-10-25 | 1949-09-13 | Du Pont | Process for preparing cadmium sulfoselenide pigments |
| US2819175A (en) * | 1954-07-15 | 1958-01-07 | Bayer Ag | New cadmium sulfide yellow pigments |
| US3527649A (en) * | 1967-12-06 | 1970-09-08 | Hercules Inc | Cadmium sulfide or cadmium sulfoselenide colored glazes and process for producing same |
| US3542526A (en) * | 1968-11-26 | 1970-11-24 | Hercules Inc | Cadmium sulfo-selenide pigments |
| GB2033418A (en) * | 1978-09-21 | 1980-05-21 | Johnson Matthey Co Ltd | Stabilised Cadmium Pigments |
| JPS58102577A (en) * | 1981-12-14 | 1983-06-18 | Canon Inc | Manufacture of light conducting cdsse |
| DE3215319A1 (en) * | 1982-04-23 | 1983-10-27 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Process for producing cadmium sulphide selenide (CdSxSe1-x) mixed crystal layers |
| JPS60161332A (en) * | 1984-01-31 | 1985-08-23 | Canon Inc | Manufacture of cadmium sulfoselenide for electrophotography |
| CN1401707A (en) * | 2001-08-16 | 2003-03-12 | 尹彦征 | High-temp-resistant cadmium sulfoselenide crimson pigment for ceramic glaze, and producing method thereof |
| CN101200604A (en) * | 2007-08-07 | 2008-06-18 | 中国科学院长春应用化学研究所 | Tin-doped (IV) sulfide lanthanum pigment and preparation method thereof |
| CN101302360A (en) * | 2008-06-27 | 2008-11-12 | 曹建荣 | Preparation of color ceramic hollow micro-bead pigment-filler |
| CN101786902A (en) * | 2010-03-04 | 2010-07-28 | 陕西科技大学 | Preparation method for extended red ZrSiO_4-Cd (S_xSe_(1-x)) pigment |
| CN103771355A (en) * | 2014-01-05 | 2014-05-07 | 吉林化工学院 | Simple solvothermal method for synthesizing CdS1/2Se1/2 nanospheres |
| 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 |
-
2016
- 2016-03-28 CN CN201610176268.XA patent/CN105838112A/en active Pending
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2482006A (en) * | 1946-10-25 | 1949-09-13 | Du Pont | Process for preparing cadmium sulfoselenide pigments |
| US2819175A (en) * | 1954-07-15 | 1958-01-07 | Bayer Ag | New cadmium sulfide yellow pigments |
| US3527649A (en) * | 1967-12-06 | 1970-09-08 | Hercules Inc | Cadmium sulfide or cadmium sulfoselenide colored glazes and process for producing same |
| US3542526A (en) * | 1968-11-26 | 1970-11-24 | Hercules Inc | Cadmium sulfo-selenide pigments |
| GB2033418A (en) * | 1978-09-21 | 1980-05-21 | Johnson Matthey Co Ltd | Stabilised Cadmium Pigments |
| JPS58102577A (en) * | 1981-12-14 | 1983-06-18 | Canon Inc | Manufacture of light conducting cdsse |
| DE3215319A1 (en) * | 1982-04-23 | 1983-10-27 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Process for producing cadmium sulphide selenide (CdSxSe1-x) mixed crystal layers |
| JPS60161332A (en) * | 1984-01-31 | 1985-08-23 | Canon Inc | Manufacture of cadmium sulfoselenide for electrophotography |
| CN1401707A (en) * | 2001-08-16 | 2003-03-12 | 尹彦征 | High-temp-resistant cadmium sulfoselenide crimson pigment for ceramic glaze, and producing method thereof |
| CN101200604A (en) * | 2007-08-07 | 2008-06-18 | 中国科学院长春应用化学研究所 | Tin-doped (IV) sulfide lanthanum pigment and preparation method thereof |
| CN101302360A (en) * | 2008-06-27 | 2008-11-12 | 曹建荣 | Preparation of color ceramic hollow micro-bead pigment-filler |
| CN101786902A (en) * | 2010-03-04 | 2010-07-28 | 陕西科技大学 | Preparation method for extended red ZrSiO_4-Cd (S_xSe_(1-x)) pigment |
| CN103771355A (en) * | 2014-01-05 | 2014-05-07 | 吉林化工学院 | Simple solvothermal method for synthesizing CdS1/2Se1/2 nanospheres |
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| SOPHIA KLOKISHNER ET AL.: "A vibronic model for the absorption spectra of Cr2+ ions in CdSexS1−x", 《J. PHYS.: CONDENS. MATTER》 * |
| U.N. ROY ET AL.: "Growth of Undoped and Chromium-Doped CdSxSe1-x Crystals by the Physical Vapor Transport Method", 《JOURNAL OF ELECTRONIC MATERIALS》 * |
| 俞康泰等: "硫硒化镉―硅酸锆包裹色料形成机理的研究", 《陶瓷学报》 * |
| 邵明梁等: "锆英石包裹硫硒化镉颜料的制备", 《陶瓷研究》 * |
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Application publication date: 20160810 |