CN102515853B - Preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment - Google Patents
Preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment Download PDFInfo
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- CN102515853B CN102515853B CN 201110453141 CN201110453141A CN102515853B CN 102515853 B CN102515853 B CN 102515853B CN 201110453141 CN201110453141 CN 201110453141 CN 201110453141 A CN201110453141 A CN 201110453141A CN 102515853 B CN102515853 B CN 102515853B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000001054 red pigment Substances 0.000 title claims abstract description 16
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 16
- GTEKSTCUDTWNPS-UHFFFAOYSA-N S.[Se-2].[SeH2].[Cd+2] Chemical compound S.[Se-2].[SeH2].[Cd+2] GTEKSTCUDTWNPS-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- 239000000701 coagulant Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000003929 acidic solution Substances 0.000 claims description 8
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 8
- 239000003637 basic solution Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 230000002040 relaxant effect Effects 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000001879 gelation Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000000049 pigment Substances 0.000 abstract description 9
- 229910052793 cadmium Inorganic materials 0.000 abstract description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000011241 protective layer Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract 3
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 239000003086 colorant Substances 0.000 abstract 1
- 238000004040 coloring Methods 0.000 abstract 1
- PGWFQHBXMJMAPN-UHFFFAOYSA-N ctk4b5078 Chemical compound [Cd].OS(=O)(=O)[Se]S(O)(=O)=O PGWFQHBXMJMAPN-UHFFFAOYSA-N 0.000 description 9
- 239000013078 crystal Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000005034 decoration Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- BKQMNPVDJIHLPD-UHFFFAOYSA-N OS(=O)(=O)[Se]S(O)(=O)=O Chemical compound OS(=O)(=O)[Se]S(O)(=O)=O BKQMNPVDJIHLPD-UHFFFAOYSA-N 0.000 description 1
- ZQRRBZZVXPVWRB-UHFFFAOYSA-N [S].[Se] Chemical compound [S].[Se] ZQRRBZZVXPVWRB-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000007516 brønsted-lowry acids Chemical class 0.000 description 1
- 150000007528 brønsted-lowry bases Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000000485 pigmenting effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- IMNMWKFKHDPTSB-UHFFFAOYSA-N silicic acid zirconium Chemical compound [Zr].[Si](O)(O)(O)O IMNMWKFKHDPTSB-UHFFFAOYSA-N 0.000 description 1
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- Glass Compositions (AREA)
- Silicon Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment, which comprises the following steps that: acid and alkaline solution is first prepared; then gel is synthesized; ingredients are dried; a cadmium red pigment protective layer zirconium silicate is generated after calcination and synthesis; acid and alkali treatment is carried out, and cadmium red pigment which is not wrapped is removed by acid and alkali, so that the product coloring quality is not affected when the pigment is used in high-temperature glaze. The preparation method of the zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment solves the problems of the prior art that the sintering temperature is quite high and the synthesis time is quite long, the prepared bright red pigment has bright colors, the washing time and the synthesis time are shortened, the preparation cost is low, and wide market prospect is realized.
Description
Technical field
The present invention relates to the pigment technology field, relate in particular to a kind of preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment.
Background technology
Along with the fast development of ceramic industry, people improve constantly the requirement of ceramic decoration, bright-coloured large red demand sharp increase, and the domestic and international market prospect is boundless.
High temperature parcel serial pigment is that the unsettled sulphur selenium flower of zirconium silicate parcel high temperature cadmium mixed crystal forms stable, chromatic colour, thoroughly solve domestic since the situation of import.Cadmium sulfoselenide pigment is unique pigment that can produce bright red tone in beramic color, the cadmium sulfoselenide pigmenting power is strong, rich color, for a long time, playing the part of important role in ceramic decoration always, but the cadmium sulfoselenide poor heat stability, oxygenolysis very easily at high temperature, how to obtain resistant to elevated temperatures large red is the problem of ceramic decoration technician research always.
Produce cadmium sulfoselenide pigment in prior art by the peritectoid method, the several different methods such as clincker process have more successfully improved the use temperature of cadmium sulfoselenide, the red pigment that has synthesized zirconium silicate parcel cadmium sulfoselenide, but its sintering temperature is higher, generated time is longer, cause preparation condition harshness and high cost, therefore, develop a kind of can be under lesser temps and low cost the red pigment of synthetic silicic acid zirconium parcel cadmium sulfoselenide have preferably that Economic Application is worth.
Summary of the invention
The objective of the invention is, the problem that exists for prior art provides a kind of zirconium silicate parcel high-sulfur selenium to spend the preparation method of cadmium crimson pigment, has solved the existing sintering temperature of prior art higher, the problem that generated time is long.
Technical scheme of the present invention is as follows: a kind of preparation method of zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment is characterized in that: described method comprises the steps:
A, by following component (weight percent) preparation acidic solution:
Cadmium Sulphate: basic zirconium chloride: water=(5%～10%): (20%～30%): (65%～73%);
B, by following component (weight percent) preparation basic solution:
Sodium sulphite: caustic soda: selenium powder: water=(6%～16%): (8%～19%): (0.5%～8%): (73%～85%);
C, coagulant liquid are synthetic: under whipped state, acidic solution and basic solution being added drop-wise to reactor simultaneously, controlling pH value is 7.5～8.5;
D, silicon gelation: coagulant liquid filter cake after filtering, add the water making beating, add water glass to reactor when stirring, wherein by weight percentage, coagulant liquid: water glass: water=(55%～65%): (30%～40%): (5%～15%), then add dilute sulphuric acid neutralization solution pH value to 7, washing and filtering;
E, oven dry batching: the silicon gel is in 110 degree oven dry, allocate lithium fluoride into, Neutral ammonium fluoride and Sodium Silicofluoride, by weight percentage, its ratio is: silicon gel: lithium fluoride: Neutral ammonium fluoride: Sodium Silicofluoride=(85%～89%): (6%～10%): (1%～2%): (4%～5%), mix grinding is even, the dress crucible;
F, calcining are synthesized: the sealing of crucible glaze slip, and 1100 degree are put into calcining furnace, 1050 degree calcinings 1 hour, the taking-up crucible, material is sent into ball mill and is crushed to 250 orders;
G, acid-alkali treatment: concentrated nitric acid is added the acid-respons still, add 250 purpose fineves when stirring, reaction adds the vitriol oil to prepare acid fines after relaxing, described acid fines weight percent is: (concentrated nitric acid: fines: the vitriol oil=30%:50%:20%), wash, be filtered to the PH=7 left and right, filter material is placed in the alkaline purification groove processes; By weight percentage, filter material: sodium hydroxide=75%:25% mixes, stirs after 1 hour, washes, and is washed till PH=6.5, and then press filtration, and oven dry under 130 degree, packing.
Beneficial effect of the present invention is: after the present invention adopts technique scheme, adopt the gel process under the highly basic condition, shortened washing time, generated time shortens, and preparation cost is low, has market outlook widely.
Embodiment
The invention provides a kind of preparation method of zirconium silicate parcel high-sulfur selenium flower cadmium crimson pigment, its technological principle is: in the generation temperature of cadmium sulfoselenide mixed crystal and glaze, the generation temperature of stable and transparent zirconium silicate differs greatly, when high temperature is synthetic, the reaction of two generations does not occur in both, the unsettled cadmium sulfoselenide mixed crystal of high temperature, wrap immediately in not participating in the zirconium silicate crystal of mixed crystal and (form and coat), thereby the high-temperature stability of the color characteristic that cadmium sulfoselenide is good and zirconium silicate combines, and obtains stable large red (pigment).Its processing step mainly comprises:
One, gel synthesizing section: selenium powder dissolving, chromium gel formation, high gel formation and silicon gel formation.
Two, oven dry ingredient station: the gel after the washing oven dry is pulverized.
Three, calcining synthesizing section: the generation of cadmium red pigment, the generation of protective layer zirconium silicate, coating process.
Four, acid-alkali treatment workshop section: will dispose with bronsted lowry acids and bases bronsted lowry less than the cadmium red pigment of parcel, affect the product tinctorial quality when avoiding using in high melting glaze.
For making purpose of the present invention, technical scheme and advantage clearer, clear and definite, the present invention is described in more detail by the following examples.
Embodiment 1:
Step 1, by following component (weight percent) preparation acidic solution: Cadmium Sulphate is water-soluble, mix with zirconium oxychloride aqueous solution, wherein Cadmium Sulphate: basic zirconium chloride: water=6%:22%:72%.
Step 2, preparation basic solution: sodium sulphite is soluble in water, add caustic soda and selenium powder in 20-40 ℃ of stirring and dissolving, optimum temps is controlled at 30 ℃, wherein sodium sulphite: caustic soda: selenium powder: water=6.5%:8.5%:1%:84%.
Step 3, coagulant liquid synthesize: acidic solution and basic solution with preparation under whipped state are added drop-wise in the reactor that includes suitable quantity of water simultaneously, and controlling pH value is that 7.5 to 8.5. best pH values are 8.
Step 4, silicon gelation: coagulant liquid filter cake after filtering, add the water making beating, stir and added water glass to reactor in 2 hours, wherein by weight percentage, coagulant liquid: water glass: water=55:35%:10%, namely take the coagulant liquid of 412.5 kilograms, the water that adds 75 kilograms stirs and added 262.5 kilograms of water glass in 2 hours, then stirs the sulfuric acid that added 45 kilograms in 2 hours, neutralization solution pH value to 7, washing and filtering.
Step 5, oven dry batching: the silicon gel is allocated lithium fluoride in 110 ℃ of oven dry, Neutral ammonium fluoride and Sodium Silicofluoride, and by weight percentage, its ratio is: silicon gel: lithium fluoride: Neutral ammonium fluoride: Sodium Silicofluoride=88%:6%:2%:4%, mix grinding be rear dress crucible evenly.
Step 6, calcining are synthesized: the sealing of crucible glaze slip, put into calcining furnace for 1100 ℃, and calcined 1 hour for 1050 ℃, take out crucible, material is sent into ball mill and is crushed to 250 orders.
Step 7, acid-alkali treatment: the concentrated nitric acids of 300 kilograms are added the acid-respons still, add 250 purpose fineves after 500 kilograms of calcinings when stirring, after relaxing, reaction adds the vitriol oil of 200 kilograms in batches, washing, filtration, process at the alkaline purification groove with 250 kilograms of NAOH, washing is filtered, 130 ℃ of oven dry obtain required Red pigment, package spare.
Embodiment 2:
Step 1, by following component (weight percent) preparation acidic solution: Cadmium Sulphate is water-soluble, mix with zirconium oxychloride aqueous solution, wherein Cadmium Sulphate: basic zirconium chloride: water=10%:23%:67%.
Step 2, preparation basic solution: sodium sulphite is soluble in water, add caustic soda and selenium powder in 20-40 ℃ of stirring and dissolving, optimum temps is controlled at 30 ℃, wherein sodium sulphite: caustic soda: selenium powder: water=6.5%:8.5%:1%:84%.
Step 3, coagulant liquid synthesize: acidic solution and basic solution with preparation under whipped state are added drop-wise in the reactor that includes suitable quantity of water simultaneously, and controlling pH value is 8.
Step 4, with the step 4 of embodiment 1.
Step 5, oven dry batching: the silicon gel is allocated lithium fluoride in 110 ℃ of oven dry, Neutral ammonium fluoride and Sodium Silicofluoride, and by weight percentage, its ratio is: silicon gel: lithium fluoride: Neutral ammonium fluoride: Sodium Silicofluoride=85%:9%:1%:5%, mix grinding be rear dress crucible evenly.
Step 6, with the step 6 of embodiment 1.
Step 7, acid-alkali treatment: the concentrated nitric acids of 300 kilograms are added the acid-respons still, add 250 purpose fineves after 500 kilograms of calcinings when stirring, after relaxing, reaction adds the vitriol oil of 200 kilograms in batches, washing, filtration, process at the alkaline purification groove with 250 kilograms of NAOH, washing is filtered, 130 ℃ of oven dry obtain required Red pigment, package spare.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (1)
1. the preparation method of a zirconium silicate wrapped high-temperature sulfur cadmium selenide bright red pigment, it is characterized in that: described method comprises the steps:
A, by following component (weight percent) preparation acidic solution:
Cadmium Sulphate: basic zirconium chloride: water=(5%～10%): (20%～30%): (65%～73%);
B, by following component (weight percent) preparation basic solution:
Sodium sulphite: caustic soda: selenium powder: water=(6%～16%): (8%～19%): (0.5%～8%): (73%～85%);
C, coagulant liquid are synthetic: under whipped state, acidic solution and basic solution being added drop-wise to reactor simultaneously, controlling the pH value is 7.5～8.5;
D, silicon gelation: coagulant liquid filter cake after filtering, add the water making beating, add water glass to reactor when stirring, wherein by weight percentage, coagulant liquid: water glass: water=(55%～65%): (30%～40%): (5%～15%), then add dilute sulphuric acid neutralization solution pH value to 7, washing and filtering;
E, oven dry batching: the silicon gel is in 110 degree oven dry, allocate lithium fluoride into, Neutral ammonium fluoride and Sodium Silicofluoride, by weight percentage, its ratio is: silicon gel: lithium fluoride: Neutral ammonium fluoride: Sodium Silicofluoride=(85%～89%): (6%～10%): (1%～2%): (4%～5%), mix grinding is even, the dress crucible;
F, calcining are synthesized: the sealing of crucible glaze slip, and 1100 degree are put into calcining furnace, 1050 degree calcinings 1 hour, the taking-up crucible, material is sent into ball mill and is crushed to 250 orders;
G, acid-alkali treatment: concentrated nitric acid is added the acid-respons still, add 250 purpose fineves when stirring, reaction adds the vitriol oil to prepare acid fines after relaxing, described acid fines weight percent is: concentrated nitric acid: fines: the vitriol oil=30% ﹕ 50% ﹕ 20%, wash, be filtered to pH=7, filter material is placed in the alkaline purification groove processes; By weight percentage, filter material: sodium hydroxide=75%:25% mixes, stirs after 1 hour, washes, and is washed till pH=6.5, and then press filtration, and oven dry under 130 degree, packing.
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| CN103159505B (en) * | 2013-03-29 | 2014-12-31 | 佛山市南海万兴材料科技有限公司 | Process for preparing zirconium-cadmium-selenium series colorant from recycled cadmium-containing wastewater |
| CN103145451A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Zirconium silicate coated cadmium yellow ceramic pigment and preparation method thereof |
| CN104671830B (en) * | 2015-03-23 | 2016-06-29 | 济南大学 | A kind of preparation method of water solublity red ceramic glaze |
| CN105000910B (en) * | 2015-05-29 | 2018-04-03 | 醴陵市科兴实业有限公司 | A kind of acid soak is containing cadmium, the direct recoverying and utilizing method of selenium acid pickle |
| CN106349799B (en) * | 2016-09-21 | 2019-05-17 | 江西金环颜料有限公司 | A kind of preparation method of coating use/ceramic ink jet printing high temperature environment-friendly type time nanometer zirconium silicate package cadmium pigment |
| CN110628243B (en) * | 2019-09-02 | 2021-06-22 | 广东道氏技术股份有限公司 | Superfine coated cadmium sulfoselenide ceramic pigment and preparation method thereof |
| CN113072839B (en) * | 2021-03-11 | 2023-01-03 | 龙南鑫坤无机新材料有限公司 | Bright bright scarlet coating pigment for ceramic ink-jet printing and preparation method thereof |
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| CN1044595C (en) * | 1994-11-17 | 1999-08-11 | 山东省硅酸盐研究设计院 | Leadless cadmiumless ceramic glazing pigment |
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