CN106280551A - The preparation method of a kind of compound coated red pigment cerium sulphide and prepared product thereof - Google Patents
The preparation method of a kind of compound coated red pigment cerium sulphide and prepared product thereof Download PDFInfo
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- CN106280551A CN106280551A CN201610679780.6A CN201610679780A CN106280551A CN 106280551 A CN106280551 A CN 106280551A CN 201610679780 A CN201610679780 A CN 201610679780A CN 106280551 A CN106280551 A CN 106280551A
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- 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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- 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
- C09C3/063—Coating
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention discloses the preparation method of a kind of compound coated red pigment cerium sulphide, first will contain γ Ce2S3The toner suspension of toner uses containing Zr4+Solution hydrolysis, hydrolyzate dry after prepare once parcel presoma powder；Then will once wrap up precursor pulp suspension to use containing Si4+Solution hydrolysis, hydrolyzate dry after prepare secondary capsulation presoma powder；By secondary capsulation presoma powder calcination processing under nonoxidizing atmosphere, i.e. prepare and there is zirconium oxide/silicon oxide compound coating layer, the compound coated red pigment cerium sulphide of parcel densification.Additionally disclose the product utilizing above-mentioned preparation method to prepare.The present invention is by the compound parcel of fractional hydrolysis so that react easily controllable, improves the effective parcel to cerium sulphide surface, and preparation process is reliable and stable, is conducive to obtaining the red pigment cerium sulphide that clad is fine and close, compact.Preparation is simple for the present invention, and obtained product stability is strong, is suitable for industrialization promotion.
Description
Technical field
The present invention relates to inorganic pigment technical field, particularly relate to the preparation method of a kind of coated red pigment cerium sulphide
And the product prepared.
Background technology
Cerium sulphide (γ-Ce2S3) red pigment is a kind of in deep-red coloration, there is brilliant angle value, strong tinting strength, tinting power, hide by force
Power also can absorb the non-toxic inorganic red pigment of ultraviolet, strongly therefore, in recent years as the replacement face of poisonous cadmium-selenium red
Expect and become study hotspot.But, temperature stability and the chemical stability of cerium sulphide colorant are poor, 350 DEG C i.e. start by
Aoxidizing and lose color development ability, being the most easily decomposed discharges H2S gas.These shortcomings of cerium sulphide colorant are significantly
Limiting its range of application, especially in Production of Ceramics, under hot conditions, its poor colour stability significantly limit it
Use as ceramic pigment.For above-mentioned situation, prior art research uses technique for packing at cerium sulphide colorant Surface coating
Resistant to elevated temperatures stability transparency material such as Zirconium orthosilicate., ZrO2Deng, its high-temperature oxidation resistant energy of coated cerium sulphide colorant obtained
Power has had and has been obviously improved.Current research, mainly uses sluggish precipitation or carries out under hydrothermal conditions at cladding
Reason, but difficulty is big, reaction controlling is difficult, the problem of product integument compactness difference to remain parcel in preparation process,
Thus have impact on reliability and the stability of product producing preparation, bring not for industrialized promotion and application
Profit.Therefore, it is badly in need of the parcel technology of preparing that research and development are new, to solve existing research and to produce institute's produced problem, thus has
It is beneficial to promote application and the development of coated red pigment cerium sulphide technology.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that one has zirconium oxide/silicon oxide compound coating
The preparation method of the coated red pigment cerium sulphide of layer, by fractional hydrolysis-compound parcel so that react easily controllable, and
Improve the effective parcel to cerium sulphide surface so that preparation process is reliable and stable, be conducive to obtaining clad fine and close, compact
Red pigment cerium sulphide.Another object of the present invention is to provide the product utilizing above-mentioned preparation method to prepare.
The purpose of the present invention is achieved by the following technical programs:
The preparation method of a kind of compound coated red pigment cerium sulphide that the present invention provides, comprises the following steps:
(1) a hydrolysis material solution is prepared
Toner suspension: by γ-Ce2S3Toner, dispersant, dehydrated alcohol, deionized water are blended and dispersed, regulation
Solution ph is alkalescence, and prepares toner suspension；
Zirconium source liquid: containing Zr4+Liquid flux；
Hydrolysis auxiliary agent: acetic acid, sodium hydroxide, sodium acetate, potassium hydroxide or ammonium acetate are dissolved in deionized water and prepare
Concentration is the hydrolysis auxiliary agent of 1～4mol/L；
(2) preparation once parcel presoma powder
According to mol ratio Zr4+∶γ-Ce2S3=1～10: 1～2, described zirconium source liquid is mixed homogeneously with toner suspension and
Obtain containing zirconium toner suspension；By volume hydrolyze auxiliary agent: by quality γ-Ce2S3Toner=1～10ml: 0.1～1g, by described water
Enzymolysis auxiliary agent joins containing stirring the reaction that is hydrolyzed in zirconium toner suspension, and product is cleaned, the most once wrapped up
Presoma powder；
(3) secondary hydrolysis material solution is prepared
Once parcel precursor pulp suspension: will once wrap up presoma powder, dispersant, dehydrated alcohol, deionization
Water is blended and dispersed, and regulation solution ph is alkalescence, prepares once parcel precursor pulp suspension；
Silicon source solution: by Si4+Silicon source and ethanol are mixed to prepare silicon source solution；
(4) secondary capsulation presoma powder is prepared
According to mol ratio Si4+∶γ-Ce2S3=1～3: 1～2, described silicon source solution is joined and once wraps up presoma
Stirring the reaction that is hydrolyzed in powder suspension liquid, product is cleaned, is obtained secondary capsulation presoma powder after drying；
(5) calcination processing of secondary capsulation presoma powder
By described secondary capsulation presoma powder calcination processing under nonoxidizing atmosphere, i.e. prepare and there is zirconium oxide/oxidation
The compound coated red pigment cerium sulphide that silicon compound coating layer, parcel are fine and close.
Further, in step of the present invention (2), the temperature of hydrolysis is 20～50 DEG C, and hydrolysis time is 1
～6h；In described step (4), the temperature of hydrolysis is 30～90 DEG C, and hydrolysis time is 2～16h.In described step (2)
Hydrolysis auxiliary agent joins containing in zirconium toner suspension with the speed of 0.02～0.2ml/min；In described step (4) silicon source solution with
The speed of 0.02～0.15ml/min joins once in parcel precursor pulp suspension.
Further, in step of the present invention (1), the consumption of dispersant is γ-Ce2S3The 5～15wt% of toner；Toner
The concrete mode using following twice dispersing of preparation of suspension is carried out: by γ-Ce2S3Toner and dispersant join anhydrous second
The mixed solution of alcohol and deionized water once disperses ,-the Ce of γ in mass ratio2S3Toner: dehydrated alcohol: deionized water=1
～8: 75～250: 200～800, after stirring ageing, centrifugal treating obtains pretreatment to remove unnecessary dispersant and impurity
Colorant；Then described pretreatment colorant is joined again and dehydrated alcohol carries out twice dispersing, in mass ratio dehydrated alcohol:
γ-Ce2S3Toner=500～600: 1～8, it is 9.0～13.0 that dispersed with stirring regulates solution ph the most afterwards, and prepares toner and hang
Supernatant liquid.
Further, in step of the present invention (3) consumption of dispersant be once parcel presoma powder 5～
15wt%；The most once parcel presoma powder: dehydrated alcohol: deionized water=1～8: 75～250: 200～800, adjusts
Joint solution ph is 9.0～13.0；Described silicon source solution is according to mass ratio Si4+Silicon source: by volume ethanol=1g: 5～8ml.
In such scheme, dispersant of the present invention is cetyl trimethylammonium bromide (CTAB), polyvinylpyrrolidine
Ketone (PVP) or Polyethylene Glycol (PEG)；Described zirconium source liquid is that propanol zirconium, butanol zirconium, zirconium sulfate aqueous solution, zirconium oxychloride are water-soluble
Liquid or acetic acid zirconium；Described Si4+Silicon source is tetraethyl orthosilicate (TEOS), sodium silicate or Ludox.
In such scheme, in step of the present invention (4), nonoxidizing atmosphere is according to volume ratio hydrogen: argon=1: 5～
The mixed atmosphere of 10, calcining heat is 600～1100 DEG C.Further, double layer aluminium oxide crucible is used to carry out calcination processing, institute
Stating its lower floor of crucible and place secondary capsulation presoma powder, aerobic substance is placed on its upper strata, such as cerium sulphide toner raw material；
The present invention utilizes the product that the preparation method of above-mentioned compound coated red pigment cerium sulphide prepares, by γ-Ce2S3
Toner and be wrapped in the zirconium oxide on its surface/silicon oxide compound coating layer transparent shell and constitute, described compound coating layer is transparent
The average thickness of housing is 30～80nm.
The method have the advantages that
(1) present invention is by fractional hydrolysis-compound parcel, improves the effective parcel to cerium sulphide colorant surface, reaction
Easily controllable, preparation process is reliable and stable, calcines in conjunction with nonoxidizing atmosphere, is effectively increased zirconium oxide/silicon oxide compound coating
The consistency of layer.
(2) zirconium oxide of the present invention/silicon oxide compound coating layer is fine and close, compact, significantly to the parcel of cerium sulphide toner particle
Improve Sprouting resistance and the high-temperature oxidation resistance of cerium sulphide colorant, at a temperature of 550 DEG C, still present red appearance, greatly expand
Its application.
(3) preparation is simple for the present invention, and obtained product stability is strong, is suitable for industrialization promotion.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail:
Fig. 1 is transmission electron microscope picture (a, b of the compound coated red pigment cerium sulphide prepared by the embodiment of the present invention one
Picture for zones of different).
Detailed description of the invention
Embodiment one:
The preparation method of a kind of compound coated red pigment cerium sulphide of the present embodiment, its step is as follows:
(1) a hydrolysis material solution is prepared
Toner suspension: by 0.5g γ-Ce2S3Toner adds with 0.05g dispersant cetyl trimethylammonium bromide (CTAB)
Entering in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, be aged 24h under magnetic agitation, centrifuge washing once removes
Unnecessary dispersant and impurity and obtain pretreatment colorant；Then pretreatment colorant is joined 75ml dehydrated alcohol, magnetic again
Power stirring supersound process are to carry out twice dispersing, and dispersed with stirring adds the sodium hydrate regulator solution pH value of 1mol/L the most afterwards
It is 12, and prepares toner suspension；
Zirconium source liquid: using 1ml butanol zirconium as zirconium source solution；
Hydrolysis auxiliary agent: 0.55g anhydrous sodium acetate is dissolved in 5ml deionized water and prepares hydrolysis auxiliary agent；
(2) preparation once parcel presoma powder
Above-mentioned zirconium source liquid is mixed homogeneously with toner suspension, ultrasonic disperse 5min and obtain containing zirconium toner suspension；Adopt
Hydrolysis auxiliary agent dropped to containing in zirconium toner suspension with peristaltic pump with the speed of 0.025ml/min, at 30 DEG C of hydrolysis temperatures, slow
Hydrolysis 2h under speed magnetic agitation, product centrifuge washing, is the most once wrapped up presoma in 95 DEG C of baking ovens
Powder；
(3) secondary hydrolysis material solution is prepared
Once parcel precursor pulp suspension: 0.5g is once wrapped up presoma powder and 0.05g dispersant hexadecane
Base trimethylammonium bromide (CTAB) joins in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, and magnetic agitation also surpasses
Sound dispersion 5min, the ammonia regulation solution ph adding 6% is 10.5, prepares once parcel precursor pulp suspension；
Silicon source solution: 0.6g tetraethyl orthosilicate is dissolved in 3.5ml dehydrated alcohol and prepares silicon source solution；
(4) secondary capsulation presoma powder is prepared
Peristaltic pump is used to drop to once wrap up presoma powder suspension by above-mentioned silicon source solution with the speed of 0.1ml/min
In liquid, hydrolysis 6h under 50 DEG C of hydrolysis temperatures, at a slow speed magnetic agitation, product centrifuge washing, dry in 95 DEG C of baking ovens
Secondary capsulation presoma powder is obtained after dry；
(5) calcination processing of secondary capsulation presoma powder
Using double layer aluminium oxide crucible, above-mentioned secondary capsulation forerunner's powder is placed by its lower floor, and one layer of sulfuration is laid on its upper strata
Cerium raw material is to consume unnecessary oxygen；Using the mixed atmosphere of volume ratio hydrogen argon=1 8 as nonoxidizing atmosphere, by room temperature
～700 DEG C, programming rate is 5 DEG C/min, after insulation 30min, is further continued for being warming up to 1000 DEG C with 5 DEG C/min and being incubated 2h, so
After be cooled to 700 DEG C with the speed of 5 DEG C/min after naturally cool to room temperature, i.e. prepare there is zirconium oxide/silicon oxide compound coating
The compound coated red pigment cerium sulphide that layer, parcel are fine and close.
As it is shown in figure 1, there is fine and close compound of zirconium oxide/silicon oxide compound coating layer, parcel prepared by the present embodiment
Coated red pigment cerium sulphide, has dense uniform, transparent clad housing, clad housing on cerium sulphide colorant surface
Average thickness be 60nm.
Embodiment two:
The preparation method of a kind of compound coated red pigment cerium sulphide of the present embodiment, its step is as follows:
(1) a hydrolysis material solution is prepared
Toner suspension: by 0.5g γ-Ce2S3Toner adds with 0.05g dispersant cetyl trimethylammonium bromide (CTAB)
Entering in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, be aged 24h under magnetic agitation, centrifuge washing once removes
Unnecessary dispersant and impurity and obtain pretreatment colorant；Then pretreatment colorant is joined 75ml dehydrated alcohol, magnetic again
Power stirring supersound process are to carry out twice dispersing, and dispersed with stirring adds the sodium hydrate regulator solution pH value of 1mol/L the most afterwards
It is 12.5, and prepares toner suspension；
Zirconium source liquid: using 1ml butanol zirconium as zirconium source solution；
Hydrolysis auxiliary agent: compound concentration is that the acetum of 2mol/ is as hydrolysis auxiliary agent；
(2) preparation once parcel presoma powder
Above-mentioned zirconium source liquid is mixed homogeneously with toner suspension, ultrasonic disperse 5min and obtain containing zirconium toner suspension；Adopt
With the speed of 0.02ml/min, 2ml hydrolyzed auxiliary agent with peristaltic pump and drops to containing in zirconium toner suspension, 45 DEG C of hydrolysis temperatures,
Hydrolysis 3h under magnetic agitation at a slow speed, product centrifuge washing, is the most once wrapped up forerunner in 95 DEG C of baking ovens
Body powder；
(3) secondary hydrolysis material solution is prepared
Once parcel precursor pulp suspension: 0.5g is once wrapped up presoma powder and 0.075g dispersant hexadecane
Base trimethylammonium bromide (CTAB) joins in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, and magnetic agitation also surpasses
Sound dispersion 5min, the ammonia regulation solution ph adding 6% is 11, prepares once parcel precursor pulp suspension；
Silicon source solution: 0.6g tetraethyl orthosilicate is dissolved in 3.5ml dehydrated alcohol and prepares silicon source solution；
(4) secondary capsulation presoma powder is prepared
Peristaltic pump is used to drop to once wrap up presoma powder suspension by above-mentioned silicon source solution with the speed of 0.1ml/min
In liquid, hydrolysis 8h under 60 DEG C of hydrolysis temperatures, at a slow speed magnetic agitation, product centrifuge washing, dry in 95 DEG C of baking ovens
Secondary capsulation presoma powder is obtained after dry；
(5) calcination processing of secondary capsulation presoma powder
Using double layer aluminium oxide crucible, above-mentioned secondary capsulation forerunner's powder is placed by its lower floor, and one layer of sulfuration is laid on its upper strata
Cerium raw material is to consume unnecessary oxygen；Using the mixed atmosphere of volume ratio hydrogen argon=1 8 as nonoxidizing atmosphere, by room temperature
～700 DEG C, programming rate is 5 DEG C/min, after insulation 30min, is further continued for being warming up to 1000 DEG C with 5 DEG C/min and being incubated 2h, so
After be cooled to 700 DEG C with the speed of 5 DEG C/min after naturally cool to room temperature, i.e. prepare there is zirconium oxide/silicon oxide compound coating
The compound coated red pigment cerium sulphide that layer, parcel are fine and close.
Embodiment three:
The preparation method of a kind of compound coated red pigment cerium sulphide of the present embodiment, its step is as follows:
(1) a hydrolysis material solution is prepared
Toner suspension: by 0.3g γ-Ce2S3Toner and 0.045g dispersant cetyl trimethylammonium bromide (CTAB)
Joining in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, be aged 24h under magnetic agitation, centrifuge washing once removes
Unnecessary dispersant and impurity is gone to obtain pretreatment colorant；Then pretreatment colorant is joined 75ml dehydrated alcohol again,
Magnetic agitation supersound process are to carry out twice dispersing, and dispersed with stirring adds the sodium hydrate regulator solution pH of 1mol/L the most afterwards
Value is 12, and prepares toner suspension；
Zirconium source liquid: using 1ml butanol zirconium as zirconium source solution；
Hydrolysis auxiliary agent: 0.52g ammonium acetate is dissolved in 2ml deionized water and prepares hydrolysis auxiliary agent；
(2) preparation once parcel presoma powder
Above-mentioned zirconium source liquid is mixed homogeneously with toner suspension, ultrasonic disperse 5min and obtain containing zirconium toner suspension；Adopt
Hydrolysis auxiliary agent dropped to containing in zirconium toner suspension with peristaltic pump with the speed of 0.025ml/min, at 50 DEG C of hydrolysis temperatures, slow
Hydrolysis 2.5h under speed magnetic agitation, product centrifuge washing, is the most once wrapped up forerunner in 95 DEG C of baking ovens
Body powder；
(3) secondary hydrolysis material solution is prepared
Once parcel precursor pulp suspension: 0.3g is once wrapped up presoma powder and 0.045g dispersant hexadecane
Base trimethylammonium bromide (CTAB) joins in the mixed solution of 25ml dehydrated alcohol and 50ml deionized water, and magnetic agitation also surpasses
Sound dispersion 5min, the ammonia regulation solution ph adding 6% is 10.5, prepares once parcel precursor pulp suspension；
Silicon source solution: 0.6g tetraethyl orthosilicate is dissolved in 3.5ml dehydrated alcohol and prepares silicon source solution；
(4) secondary capsulation presoma powder is prepared
Use peristaltic pump, with the speed of 0.15ml/min, above-mentioned silicon source solution is dropped to once wrap up presoma powder to hang
In supernatant liquid, hydrolysis 12h under 50 DEG C of hydrolysis temperatures, at a slow speed magnetic agitation, product centrifuge washing, in 95 DEG C of baking ovens
Obtain secondary capsulation presoma powder after drying；
(5) calcination processing of secondary capsulation presoma powder
Using double layer aluminium oxide crucible, above-mentioned secondary capsulation forerunner's powder is placed by its lower floor, and one layer of sulfuration is laid on its upper strata
Cerium raw material is to consume unnecessary oxygen；Using the mixed atmosphere of volume ratio hydrogen argon=1 8 as nonoxidizing atmosphere, by room temperature
～700 DEG C, programming rate is 5 DEG C/min, after insulation 30min, is further continued for being warming up to 1000 DEG C with 5 DEG C/min and being incubated 2h, so
After be cooled to 700 DEG C with the speed of 5 DEG C/min after naturally cool to room temperature, i.e. prepare there is zirconium oxide/silicon oxide compound coating
The compound coated red pigment cerium sulphide that layer, parcel are fine and close.
Compound coated red pigment cerium sulphide obtained by various embodiments of the present invention, its chromatic value is as shown in table 1.
Table 1 various embodiments of the present invention are combined the chromatic value of coated red pigment cerium sulphide
| Embodiment | L* | a* | b* |
| Embodiment one | 32.06 | 39.28 | 30.04 |
| Embodiment two | 31.44 | 38.36 | 32.12 |
| Embodiment three | 31.26 | 38.02 | 32.27 |
With the commercial cerium sulphide colorant that do not wraps up as a comparison case, the compound coated sulfur obtained by the embodiment of the present invention one
Changing cerium red pigment, in air atmosphere, the chromatic value under different calcining heats is as shown in table 2.
Table 2 embodiment of the present invention one and comparative example be the chromatic value under different calcining heats in air atmosphere
Claims (10)
1. the preparation method of a compound coated red pigment cerium sulphide, it is characterised in that comprise the following steps:
(1) a hydrolysis material solution is prepared
Toner suspension: by γ-Ce2S3Toner, dispersant, dehydrated alcohol, deionized water are blended and dispersed, regulate solution
PH value is alkalescence, and prepares toner suspension；
Zirconium source liquid: containing Zr4+Liquid flux；
Hydrolysis auxiliary agent: acetic acid, sodium hydroxide, sodium acetate, potassium hydroxide or ammonium acetate are dissolved in deionized water and prepare concentration
It it is the hydrolysis auxiliary agent of 1～4mol/L；
(2) preparation once parcel presoma powder
According to mol ratio Zr4+∶γ-Ce2S3=1～10: 1～2, described zirconium source liquid is mixed homogeneously with toner suspension and obtains
Containing zirconium toner suspension；By volume hydrolyze auxiliary agent: by quality γ-Ce2S3Toner=1～10ml: 0.1～1g, helps described hydrolysis
Agent joins containing stirring the reaction that is hydrolyzed in zirconium toner suspension, and product is cleaned, the most once wrapped up forerunner
Body powder；
(3) secondary hydrolysis material solution is prepared
Once parcel precursor pulp suspension: will once wrap up presoma powder, dispersant, dehydrated alcohol, deionized water common
Mixed and dispersed, regulation solution ph is alkalescence, prepares once parcel precursor pulp suspension；
Silicon source solution: by Si4+Silicon source and ethanol are mixed to prepare silicon source solution；
(4) secondary capsulation presoma powder is prepared
According to mol ratio Si4+∶γ-Ce2S3=1～3: 1～2, described silicon source solution is joined once parcel presoma powder and hangs
Stirring the reaction that is hydrolyzed in supernatant liquid, product is cleaned, is obtained secondary capsulation presoma powder after drying；
(5) calcination processing of secondary capsulation presoma powder
By described secondary capsulation presoma powder calcination processing under nonoxidizing atmosphere, i.e. prepare that to have zirconium oxide/silicon oxide multiple
Close clad, the compound coated red pigment cerium sulphide of parcel densification.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 1, it is characterised in that: described step
Suddenly in (2), the temperature of hydrolysis is 20～50 DEG C, and hydrolysis time is 1～6h；The temperature of hydrolysis in described step (4)
Degree is 30～90 DEG C, and hydrolysis time is 2～16h.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 1, it is characterised in that: described step
Suddenly in (2), hydrolysis auxiliary agent joins containing in zirconium toner suspension with the speed of 0.02～0.2ml/min；Silicon in described step (4)
Source solution joins once in parcel precursor pulp suspension with the speed of 0.02～0.15ml/min.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 1, it is characterised in that: described step
Suddenly in (1), the consumption of dispersant is γ-Ce2S3The 5～15wt% of toner.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 4, it is characterised in that: described step
Suddenly in (1), the preparation of toner suspension uses the mode of twice dispersing to carry out: by γ-Ce2S3Toner and dispersant join anhydrous
The mixed solution of ethanol and deionized water once disperses ,-the Ce of γ in mass ratio2S3Toner: dehydrated alcohol: deionized water
=1～8: 75～250: 200～800, after stirring ageing, centrifugal treating obtains pre-place to remove unnecessary dispersant and impurity
Reason colorant；Then described pretreatment colorant is joined again and dehydrated alcohol carries out twice dispersing, in mass ratio dehydrated alcohol:
γ-Ce2S3Toner=500～600: 1～8, it is 9.0～13.0 that dispersed with stirring regulates solution ph the most afterwards, and prepares toner and hang
Supernatant liquid.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 1, it is characterised in that: described step
Suddenly in (3), the consumption of dispersant is once to wrap up the 5～15wt% of presoma powder；The most once parcel presoma powder
: dehydrated alcohol: deionized water=1～8: 75～250: 200～800, regulation solution ph is 9.0～13.0；Described silicon source is molten
Liquid is according to mass ratio Si4+Silicon source: by volume ethanol=1g: 5～8ml.
7., according to the preparation method of the compound coated red pigment cerium sulphide described in claim 1 or 4 or 5 or 6, its feature exists
In: described dispersant is cetyl trimethylammonium bromide, polyvinylpyrrolidone or Polyethylene Glycol；Described zirconium source liquid is third
Alcohol zirconium, butanol zirconium, zirconium sulfate aqueous solution, zirconium oxychloride aqueous solution or acetic acid zirconium；Described Si4+Silicon source is tetraethyl orthosilicate, silicic acid
Sodium or Ludox.
The preparation method of compound coated red pigment cerium sulphide the most according to claim 1, it is characterised in that: described step
Suddenly in (4), nonoxidizing atmosphere is according to volume ratio hydrogen: argon=1: the mixed atmosphere of 5～10, and calcining heat is 600～1100
℃。
The preparation method of compound coated red pigment cerium sulphide the most according to claim 8, it is characterised in that: described step
Suddenly (4) use double layer aluminium oxide crucible to carry out calcination processing, and secondary capsulation presoma powder is placed by its lower floor of described crucible, its
Aerobic substance is placed on upper strata.
10. utilize the product that the preparation method of the described compound coated red pigment cerium sulphide of one of claim 1-9 prepares, its
It is characterised by: by γ-Ce2S3Toner and be wrapped in the zirconium oxide on its surface/silicon oxide compound coating layer transparent shell and constitute,
The average thickness of described compound coating layer transparent shell is 30～80nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610679780.6A CN106280551B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of compound coated red pigment cerium sulphide and its product obtained |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610679780.6A CN106280551B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of compound coated red pigment cerium sulphide and its product obtained |
Publications (2)
| Publication Number | Publication Date |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106928752A (en) * | 2017-02-28 | 2017-07-07 | 景德镇陶瓷大学 | A kind of preparation method of zirconium silicate parcel ceramic pigment with zirconium carbonate ammonium as zirconium source and its obtained product |
| CN107758720A (en) * | 2017-10-25 | 2018-03-06 | 景德镇陶瓷大学 | A kind of composite mixed γ~Ce of zirconium silicate coated low price ion2S3Red pigment and preparation method thereof |
| CN108219536A (en) * | 2017-12-12 | 2018-06-29 | 景德镇陶瓷大学 | A kind of aluminium oxide coated γ ~ Ce2S3The preparation method of red colorant and its product obtained |
| CN115386246A (en) * | 2022-09-13 | 2022-11-25 | 中山市华山高新陶瓷材料有限公司 | Preparation method of double-layer coated cerium sulfide red pigment chemical coating film |
| CN115895340A (en) * | 2022-12-29 | 2023-04-04 | 武汉山羽新材料科技有限公司 | Production method of small-particle-size coated ceramic ink material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106928752A (en) * | 2017-02-28 | 2017-07-07 | 景德镇陶瓷大学 | A kind of preparation method of zirconium silicate parcel ceramic pigment with zirconium carbonate ammonium as zirconium source and its obtained product |
| CN107758720A (en) * | 2017-10-25 | 2018-03-06 | 景德镇陶瓷大学 | A kind of composite mixed γ~Ce of zirconium silicate coated low price ion2S3Red pigment and preparation method thereof |
| CN108219536A (en) * | 2017-12-12 | 2018-06-29 | 景德镇陶瓷大学 | A kind of aluminium oxide coated γ ~ Ce2S3The preparation method of red colorant and its product obtained |
| CN108219536B (en) * | 2017-12-12 | 2020-07-10 | 景德镇陶瓷大学 | Alumina-coated gamma-Ce2S3Preparation method of red pigment |
| CN115386246A (en) * | 2022-09-13 | 2022-11-25 | 中山市华山高新陶瓷材料有限公司 | Preparation method of double-layer coated cerium sulfide red pigment chemical coating film |
| CN115386246B (en) * | 2022-09-13 | 2024-02-06 | 中山市华山高新陶瓷材料有限公司 | Preparation method of double-layer coated cerium sulfide red pigment chemical coating |
| CN115895340A (en) * | 2022-12-29 | 2023-04-04 | 武汉山羽新材料科技有限公司 | Production method of small-particle-size coated ceramic ink material |
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