CN101786902B - Preparation method for zirconium silicate wrapped cadmium sulfide selenide scarlet pigment - Google Patents
Preparation method for zirconium silicate wrapped cadmium sulfide selenide scarlet pigment Download PDFInfo
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- CN101786902B CN101786902B CN 201010117228 CN201010117228A CN101786902B CN 101786902 B CN101786902 B CN 101786902B CN 201010117228 CN201010117228 CN 201010117228 CN 201010117228 A CN201010117228 A CN 201010117228A CN 101786902 B CN101786902 B CN 101786902B
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Abstract
The invention relates to a preparation method for an extended red ZrSiO_4-Cd(S_xSe_(1-x)) pigment.When a presoma is prepared by utilizing a collosol coprecipitation method, a developing body is generated in a solution and rare-earth elements are introduced for being mixed with a colorant, thereby changing the surface activity thereof, improving the chemical affinity of the developing body and a coating, and facilitating the cladding of the presoma to the developing body; microwave hydro-thermal treatment is carried out on the presoma of the ZrSiO_4-Cd(S_xSe_(1-x)) pigment by utilizing a microwave hydro-thermal method to accelerate chemical reactions of the system; ceramic pigment crystals are dissolved out at first, and then the conditions are changed so as to dissolve out inclusion crystals by taking the firstly dissolved crystal as nucluting agent; a transitional face can be generated by materials formed by the rare-earth elements and a mineralizer in the reaction system, ludox and zirconium sol in the forming process of zirconium silicate, the crystallization activation energy of the zirconium silicate can be decreased, the crystallization speed of the zirconium silicate can bequickened, the zirconium silicate can be devitrified in shorter time and the densifying of the zirconium silicate inclusion can be ensured, thereby achieving the purpose of coating the pigment.
Description
Technical field
The present invention relates to a kind of preparation method of red colorant, be specifically related to a kind of preparation method of extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
Background technology
The large red color development of cadmium sulfoselenide is pure, bright in luster, and the color development wide ranges is to can be used at present red stain the most gorgeous in the ceramic decoration.Particularly zircon crystal packaged cadmium sulfoselenide colorant had both possessed good colouring effect, had again the characteristic of high-temperature stable concurrently, and the reputation of " Chinese red " is arranged, and was very precious red colorant.Yet because the synthesis temperature of zirconium silicate is very high, cadmium sulfoselenide is easy oxygenolysis at high temperature again, and crystal formation and the cadmium sulfoselenide of zirconium silicate are inconsistent, cause the encapsulation ratio of zirconium silicate parcel cadmium sulfoselenide pigment excessively low, synthetic cost is very high, thereby its range of application is very limited.Therefore solve at low temperatures synthetic silicic acid zirconium parcel cadmium sulfoselenide red stain, be its synthetic cost of reduction, improve one of effective way of its combined coefficient.
The method for preparing at present the large red of zirconium silicate parcel cadmium sulfoselenide mainly contains solid phase method, solution deposit, double-contracting method, hydrothermal method.Wherein: the inclusion pigment granularity that solid phase method synthesizes is large, skewness, and the encapsulation ratio of pigment is very low because selenium powder volatilizees easily, and the colorant tinctorial strength is very weak; Although solution deposit encapsulation ratio higher (8%～10%), tinctorial strength is better, and severe reaction conditions requires presoma dry through several, so that the production cycle prolongs the synthesis temperature of pigment very high (about 1200 ℃～1300 ℃).Double-contracting method production unit is complicated, operation easier is large, the production cycle is long, expensive raw material price, so that production cost is too high.Above-mentioned three kinds of methods all are unfavorable for suitability for industrialized production.Hydrothermal method is to combine with solution deposit, can directly generate the parcel phase from solution, and tinting material is wrapped up, and has reduced common wet chemistry method and need to pass through high-temperature calcination, this step that may form hard aggregation and sneak into impurity of ball milling.Because hydrothermal temperature is very low, well below CdS
xSe
1-xDecomposition temperature, this has overcome the difficult problem that toner decomposes to a great extent.
Adopting the synthetic ZrSiO of liquid phase method
4-CdS
xSe
1-xIn the research of colorant, Deng Yang (Deng Yang, Deng Jiancheng, the research of sol precipitation method synthetic silicic acid zirconium parcel cadmium sulfoselenide pigment, 2006) employing sol-coprecipitation method combines with auxiliary agent G and has synthesized zirconium silicate parcel cadmium sulfoselenide colorant, utilizes CeO
2Property and the mechanism of nucleation of the zirconium silicate large red that under 950 ℃, synthesized zirconium silicate parcel cadmium sulfoselenide, when high-temperature calcination because the decomposition of cadmium sulfoselenide, need to seal preferably iron flask container, operational difficulty, container is yielding and affect its sealing effectiveness.Yekta.B.Eftekhan, Tamizifar.M, Rahimi.N, Song Xiaolan, Peng Lin etc. adopt Cd (NO
3)
2, Se powder, ZrOCl
28H
2O, Na
2SiO
39H
2O, Na
2The soluble salts such as S are raw material, and (silicate journal, 2009,37 (7): 1267-1267), but its generated time reaches 10h, and has no the report of doping vario-property colorant to utilize conventional hydrothermal method to synthesize zirconium silicate parcel cadmium sulfoselenide colorant.
Microwave-hydrothermal method for international scope in recent years prepares a kind of novel method that nano-powder conducts a research, is compared with the powder that conventional hydrothermal method and chemical method are synthetic, has the diameter of particle narrowly distributing, good dispersity, and it is few to reunite, the advantages such as the complete and good crystallinity of crystal grain.Microwave-hydrothermal method synthesis rate and the efficiency all height than traditional hydrothermal method are a lot, and it is lower to have temperature of reaction, the characteristics that the reaction times is shorter.
Summary of the invention
The object of the present invention is to provide a kind of technology controlling and process simple, generated time is short, and synthesis temperature is low, parcel efficient is high, the narrow diameter distribution of occlusion pigment, good dispersity, it is few to reunite, and has the preparation method of the extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment of industrialization development potentiality.
For achieving the above object, the technical solution used in the present invention is: 1) at first, press CdSO
4: Na
2S: Se=1: (0.6～0.8): the mol ratio of (0.2～0.3) is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2The adding selenium powder drips simultaneously and gets NaSSe solution, wherein Se: NaOH=1 after the sodium hydroxide stirring is dissolved selenium powder fully in the S solution: 1 mol ratio, and again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution; 2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4=1: 2: 2.2 mol ratio is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, with step 1) to be added in the mixed sols pH with the acetic acid hierarchy of control constant for the cadmium sulfoselenide hanging drop that obtains, dropwise rear adjusting pH=6～9, continue to stir 1.5～2.5h, leave standstill 15～20h, suction filtration, drying is ground to get presoma; 3) microwave hydrothermal is processed: mix the mineralizer of presoma quality 0.1～3% and 1～3% soluble rare-earth salt and get mixture in described presoma, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g: 10ml with mixture and get mixing solutions, it is 60～80% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 160 ℃～200 ℃, treatment time 15～50min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder; 4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
Mineralizer of the present invention is LiF or NaF; Soluble rare-earth salt is cerous nitrate, lanthanum nitrate or europium nitrate.
Compared with prior art, when the present invention utilizes the standby presoma of sol-coprecipitation legal system, by in solution, generating developing body, introducing simultaneously rare earth element mixes to tinting material, change its surperficial surfactivity high energy, improved the chemical affinity of developing body and coating layer, be beneficial to the zirconium silicate presoma to the coating of aobvious body agent; Utilize microwave-hydrothermal method to the reaction system heating rapidly, evenly, there is not thermograde, the characteristics of acceleration system chemical reaction are carried out the microwave hydrothermal processing to the presoma of zirconium silicate parcel cadmium sulfoselenide colorant, because the colorant crystal can be separated out under different condition (pressure in the water heating kettle and temperature etc.) with the zirconium silicate crystal, the ceramic pigment crystal is separated out first, then change condition, because existing crystal exists in the water heating kettle, can as making the parcel crystal, the Nucleating Agent growth separate out take the crystal of separating out first, and the material that rare earth element and mineralizer form in reaction system can generate transition phase with silicon sol and zirconium colloidal sol in the forming process of zirconium silicate, reduce the crystallization activation energy of zirconium silicate, quickening is from the crystallization speed of zirconium silicate, be conducive to the in the short period of time densification of crystallization and zirconium silicate inclusion of zirconium silicate, and can reach the purpose with the colorant parcel.Because Microwave Heating is rapid, can significantly shorten the reaction times of conventional hydrothermal method, synthetic colorant is rapid, do not need through high-temperature heat treatment simultaneously, it is little to have a colouring agent loss, and encapsulation ratio is high, colorant narrow particle size distribution and particle diameter are little, the advantages such as colorant integument densification.
Description of drawings
Fig. 1 is for mixing 1% lanthanum nitrate 160 ℃～200 ℃ heat treated XRD figure of lower Microwave Water; Fig. 2 mixes 1% cerous nitrate to be the XRD figure of ripple hydrothermal treatment consists under 180 ℃～200 ℃; Fig. 3 is occlusion pigment lightness synthetic under differing temps, and curve 1 is for to mix 1% cerous nitrate, and curve 2 is for mixing 1% lanthanum nitrate.
Fig. 4 be occlusion pigment synthetic under the differing temps red/green value (a
*), curve 1 is for to mix 1% cerous nitrate, and curve 2 is for mixing 1% lanthanum nitrate.
Fig. 5 is the Huang/indigo plant value (b of occlusion pigment synthetic under the differing temps
*), curve 1 is for to mix 1% cerous nitrate, and curve 2 is for mixing 1% lanthanum nitrate.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:1) at first, press CdSO
4: Na
2S: Se=1: 0.6: 0.2 mol ratio is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2The adding selenium powder drips simultaneously and gets NaSSe solution, wherein Se: NaOH=1 after the sodium hydroxide stirring is dissolved selenium powder fully in the S solution: 1 mol ratio, and again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution; 2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4=1: 2: 2.2 mol ratio is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, with step 1) to be added in the mixed sols pH with the acetic acid hierarchy of control constant for the cadmium sulfoselenide hanging drop that obtains, dropwises rear adjusting pH=6, continue to stir 1.5h, leave standstill 15h, suction filtration, drying is ground to get presoma; 3) microwave hydrothermal is processed: mix the mineralizer LiF of presoma quality 1% and 1% soluble rare-earth salt cerous nitrate and get mixture in described presoma, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g: 10ml with mixture and get mixing solutions, it is 70% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 160 ℃, treatment time 15min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder; 4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
Embodiment 2:1) at first, press CdSO
4: Na
2S: Se=1: 0.8: 0.25 mol ratio is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2The adding selenium powder drips simultaneously and gets NaSSe solution, wherein Se: NaOH=1 after the sodium hydroxide stirring is dissolved selenium powder fully in the S solution: 1 mol ratio, and again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution; 2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4=1: 2: 2.2 mol ratio is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, with step 1) to be added in the mixed sols pH with the acetic acid hierarchy of control constant for the cadmium sulfoselenide hanging drop that obtains, dropwises rear adjusting pH=7, continue to stir 2h, leave standstill 18h, suction filtration, drying is ground to get presoma; 3) microwave hydrothermal is processed: mix the mineralizer NaF of presoma quality 0.1% and 2% soluble rare-earth salt lanthanum nitrate and get mixture in described presoma, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g: 10ml with mixture and get mixing solutions, it is 60% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 180 ℃, treatment time 35min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder; 4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
Embodiment 3:1) at first, press CdSO
4: Na
2S: Se=1: 0.7: 0.3 mol ratio is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2The adding selenium powder drips simultaneously and gets NaSSe solution, wherein Se: NaOH=1 after the sodium hydroxide stirring is dissolved selenium powder fully in the S solution: 1 mol ratio, and again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution; 2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4=1: 2: 2.2 mol ratio is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, with step 1) to be added in the mixed sols pH with the acetic acid hierarchy of control constant for the cadmium sulfoselenide hanging drop that obtains, dropwises rear adjusting pH=9, continue to stir 2.5h, leave standstill 20h, suction filtration, drying is ground to get presoma; 3) microwave hydrothermal is processed: mix the mineralizer LiF of presoma quality 3% and 3% soluble rare-earth salt europium nitrate and get mixture in described presoma, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g: 10ml with mixture and get mixing solutions, it is 80% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 200 ℃, treatment time 50min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder; 4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
Embodiment 4:1) at first, press CdSO
4: Na
2S: Se=1: 0.7: 0.3 mol ratio is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2The adding selenium powder drips simultaneously and gets NaSSe solution, wherein Se: NaOH=1 after the sodium hydroxide stirring is dissolved selenium powder fully in the S solution: 1 mol ratio, and again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution; 2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4=1: 2: 2.2 mol ratio is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, with step 1) to be added in the mixed sols pH with the acetic acid hierarchy of control constant for the cadmium sulfoselenide hanging drop that obtains, dropwises rear adjusting pH=8, continue to stir 2.5h, leave standstill 20h, suction filtration, drying is ground to get presoma; 3) microwave hydrothermal is processed: mix the mineralizer NaF of presoma quality 2% and 1% soluble rare-earth salt lanthanum nitrate and get mixture in described presoma, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g: 10ml with mixture and get mixing solutions, it is 80% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 200 ℃, treatment time 50min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder; 4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
As can be seen from Figure 1, under 160 ℃, 180 ℃, 200 ℃, all generated ZrSiO
4/ CdS
xSe
1-xCrystalline phase, when treatment temp is 160 ℃ and 180 ℃, ZrSiO
4/ CdS
xSe
1-xCrystal is less, has generated SiO
2Crystalline phase is at 200 ℃ of lower SiO
2Crystalline phase reduces, ZrSiO
4/ CdS
xSe
1-xCrystalline phase increases.
Fig. 2 has generated ZrSiO at 180 ℃ and 200 ℃
4/ CdS
xSe
1-xCrystalline phase, ZrSiO
4/ CdS
xSe
1-xBe eager to excel than figure one in the corresponding peak of crystalline phase, cerous nitrate is to ZrSiO
4/ CdS
xSe
1-xThe generation of crystalline phase and grow up promoter action is arranged.
Lightness increases along with the rising of temperature and all greater than 50, it is higher than the lightness of mixing lanthanum (2) to mix cerium (1) as can be seen from Figure 3.Mix the red value (a of cerium (1) among Fig. 4 and Fig. 5
*) and yellow value (b
*) at 180 ℃ a peak value is arranged, illustrate at 180 ℃ of lower synthetic occlusion pigments to have higher lightness and red value.
XRD diffraction to sum up, color difference analysis shows, has synthesized ZrSiO under 160～200 ℃
4/ CdS
xSe
1-xOcclusion pigment, the doping by rare earth element has promoted ZrSiO
4/ CdS
xSe
1-xThe generation of crystalline phase and growing up.Microwave-hydrothermal method has been synthesized zirconium silicate parcel cadmium sulfoselenide colorant within lower temperature (below 200 ℃) and very short time, the introducing of rare earth element has very large promoter action to occlusion pigment.
The present invention combines the common advantage of sol precipitation and microwave-hydrothermal method, and synthetic a kind of heatproof is high, firing range is wide, be easy to the high temperature modification ceramic decoration zirconium silicate xenocryst parcel cadmium sulfoselenide crimson pigment controlling and grasp when wide application, use.Require on the technique treatment temp low, the treatment time is short, the narrow diameter distribution of occlusion pigment, and it is few to reunite, good dispersity, the inclusion of colorant is fine and close, and the parcel defective is few.
Claims (1)
1. the preparation method of an extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment is characterized in that:
1) at first, presses CdSO
4: Na
2S:Se=1:(0.6～0.8): the mol ratio of (0.2～0.3) is with CdSO
4And Na
2S is dissolved in respectively the CdSO that is made into 0.25mol/L in the distilled water
4Na with 0.2mol/L
2S solution is then to Na
2Add selenium powder in the S solution and drip simultaneously sodium hydroxide and stir after selenium powder is dissolved fully to get NaSSe solution, Se:NaOH=1:1 mol ratio wherein is again with described CdSO
4Solution is added drop-wise to and gets cadmium sulfoselenide suspension in the NaSSe solution;
2) secondly, press CdSO
4: ZrOCl
2: Na
2SiO
4The mol ratio of=1:2:2.2 is with ZrOCl
2And Na
2SiO
4Be dissolved in respectively the ZrOCl that is made into 0.4mol/L in the distilled water
2Na with 0.48mol/L
2SiO
4Then solution adopt ammoniacal liquor or acetic acid to regulate ZrOCl
2And Na
2SiO
4The pH value of solution is both to be mixed to get mixed sols after 5～8, it is constant that the cadmium sulfoselenide hanging drop that step 1) is obtained is added in the mixed sols pH with the acetic acid hierarchy of control, dropwise rear adjusting pH=6～9, continue to stir 1.5～2.5h, leave standstill 15～20h, suction filtration, drying is ground to get presoma;
3) microwave hydrothermal is processed: mix the mineralizer LiF of presoma quality 0.1～3% or the soluble rare-earth salt cerous nitrate of NaF and 1～3% in described presoma, lanthanum nitrate or europium nitrate get mixture, under ultrasonic wave, mixture and distilled water are scattered in distilled water in the ratio of 1g:10ml with mixture and get mixing solutions, it is 60～80% that mixing solutions is placed microwave hydrothermal still control compactedness, the hydrothermal treatment consists temperature is 160 ℃～200 ℃, treatment time 15～50min, zirconium silicate generates occlusion pigment take the cadmium sulfoselenide crystal as nucleus growth, filter, drying is ground to get powder;
4) described powder is dry behind the 5mol/L chlorohydric acid pickling, grind to get extended red ZrSiO _ 4-Cd (S _ xSe _ (1-x)) pigment.
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| CN102584342A (en) * | 2012-01-13 | 2012-07-18 | 南京工业大学 | High-efficiency energy-saving preparation method for ceramic occlusion pigment |
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| CN106590031B (en) * | 2016-12-02 | 2018-07-24 | 佛山市华意陶瓷颜料有限公司 | A kind of cadmium sulfoselenide occlusion pigment, ceramic ink and preparation method thereof |
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| 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 |
| CN113479895B (en) * | 2021-07-05 | 2022-10-04 | 江西金环颜料有限公司 | Method for preparing superfine zirconium silicate and zirconium silicate-based coating pigment by one-step precipitation method |
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| 宋晓岚等.ZrSiO4/Cd(S1-xSex)包裹色料的水热合成.《硅酸盐学报》.2009,第37卷(第7期),1264-1267. * |
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