CN106280551B - A kind of preparation method of compound coated red pigment cerium sulphide and its product obtained - Google Patents
A kind of preparation method of compound coated red pigment cerium sulphide and its product obtained Download PDFInfo
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- CN106280551B CN106280551B CN201610679780.6A CN201610679780A CN106280551B CN 106280551 B CN106280551 B CN 106280551B CN 201610679780 A CN201610679780 A CN 201610679780A CN 106280551 B CN106280551 B CN 106280551B
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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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- 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 a kind of preparation methods of compound coated red pigment cerium sulphide, will contain γ Ce first2S3The toner suspension of toner, which uses, contains Zr4+Solution hydrolysis, primary package presoma powder is made after hydrolysate drying；Then it will once wrap up precursor pulp suspension and use and contain Si4+Solution hydrolysis, secondary capsulation presoma powder is made after hydrolysate drying；By secondary capsulation presoma powder under nonoxidizing atmosphere calcination processing, obtain with the fine and close compound coated red pigment cerium sulphide of zirconium oxide/silica compound coating layer, package.In addition it also discloses and utilizes product made from above-mentioned preparation method.The present invention passes through the compound package of fractional hydrolysis so that reaction is easily controllable, improves effective package to cerium sulphide surface, and preparation process is reliable and stable, is conducive to obtain clad densification, compact red pigment cerium sulphide.Preparation is simple by 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 more particularly to a kind of preparation methods of coated red pigment cerium sulphide
And its product obtained.
Background technology
Cerium sulphide (γ-Ce2S3) red pigment be a kind of is in deep-red coloration, there is brilliant angle value, strong tinting strength, tinting power, strong cover
Power and the non-toxic inorganic red pigment that ultraviolet light can be absorbed strongly, therefore, in recent years as the replacement face of toxic cadmium-selenium red
Expect and becomes research hotspot.But the temperature stability and chemical stability of cerium sulphide colorant are poor, start quilt at 350 DEG C
It aoxidizes and loses color development ability, be easily decomposed releases H in acid condition2S gases.These disadvantages of cerium sulphide colorant are significantly
It limits its scope of application, especially in Production of Ceramics, its poor colour stability significantly limits it under hot conditions
Use as ceramic pigment.For the above situation, prior art research is coated using technique for packing on cerium sulphide colorant surface
Heat safe stability transparency material such as zirconium silicate, ZrO2Deng coated cerium sulphide colorant its high-temperature oxidation resistant energy obtained
Power, which has, to be obviously improved.Current research is mainly carried out using sluggish precipitation or under hydrothermal conditions at cladding
Reason, but remain in preparation process that package difficulty is big, reaction controlling is difficult, the problem of product wrapping layer compactness difference,
To affect the stability of reliability and product prepared by production, brought not for industrialized promotion and application
Profit.Therefore, it is badly in need of researching and developing new package technology of preparing, to solve existing research and the production institute problem, to have
Conducive to the application and development of promotion coated red pigment cerium sulphide technology.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind having zirconium oxide/silica compound coating
The preparation method of the coated red pigment cerium sulphide of layer, passes through the compound package of fractional hydrolysis-so that and reaction is easily controllable, and
Improve effective package to cerium sulphide surface so that preparation process is reliable and stable, and it is fine and close, compact to be conducive to acquisition clad
Red pigment cerium sulphide.Another object of the present invention is to provide utilize product made from above-mentioned preparation method.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of compound coated red pigment cerium sulphide provided by the invention, includes the following steps：
(1) a hydrolysis material solution is prepared
Toner suspension：By γ-Ce2S3Toner, dispersant, absolute ethyl alcohol, deionized water are blended and evenly dispersed, adjusting
Toner suspension is made in alkalinity in solution ph；
Zirconium source liquid：Containing Zr4+Liquid flux；
Hydrolyze auxiliary agent：Acetic acid, sodium hydroxide, sodium acetate, potassium hydroxide or ammonium acetate are dissolved in deionized water and are made
The hydrolysis auxiliary agent of a concentration of 1~4mol/L；
(2) primary package presoma powder is prepared
According to molar ratio Zr4+∶γ-Ce2S3=1~10: 1~2, zirconium source liquid is uniformly mixed with toner suspension and
Obtain the suspension of toner containing zirconium；By volume of water enzymolysis auxiliary agent: pressing quality γ-Ce2S3Toner=1~10ml: 0.1~1g, by the water
Enzymolysis auxiliary agent is added to stirring in the suspension of toner containing zirconium and reaction is hydrolyzed, and is once wrapped up after reaction product cleaning, drying
Presoma powder；
(3) secondary hydrolysis material solution is prepared
Primary package precursor pulp suspension：Presoma powder, dispersant, absolute ethyl alcohol, deionization will once be wrapped up
Water blending is simultaneously evenly dispersed, adjusts solution ph in alkalinity, once package precursor pulp suspension is made；
Silicon source solution：By Si4+Silicon source is mixed to prepare silicon source solution with ethyl alcohol；
(4) secondary capsulation presoma powder is prepared
According to molar ratio Si4+∶γ-Ce2S3=1~3: 1~2, the silicon source solution is added to primary package presoma
Reaction is hydrolyzed in stirring in powder suspension liquid, and secondary capsulation presoma powder is obtained after reaction product cleaning, drying；
(5) calcination processing of secondary capsulation presoma powder
By the secondary capsulation presoma powder under nonoxidizing atmosphere calcination processing, obtain with zirconium oxide/oxidation
The fine and close compound coated red pigment cerium sulphide of silicon compound coating layer, package.
Further, the temperature of hydrolysis is 20~50 DEG C in step (2) of the present invention, hydrolysis time 1
~6h；The temperature of hydrolysis is 30~90 DEG C in the step (4), and hydrolysis time is 2~16h.In the step (2)
Hydrolysis auxiliary agent is added to the speed of 0.02~0.2ml/min in the suspension of toner containing zirconium；In the step (4) silicon source solution with
The speed of 0.02~0.15ml/min is added in primary package precursor pulp suspension.
Further, the dosage of dispersant is γ-Ce in step (1) of the present invention2S35~15wt% of toner；Toner
The preparation of suspension is specifically carried out by the way of following twice dispersing：By γ-Ce2S3Toner is added to anhydrous second with dispersant
Once disperseed in alcohol and the mixed solution of deionized water, in mass ratio γ-Ce2S3Toner: absolute ethyl alcohol: deionized water=1
~8: 75~250: 200~800, after stirring ageing, centrifugal treating is pre-processed with removing extra dispersant and impurity
Colorant；Then the pretreatment colorant is added to again in absolute ethyl alcohol and carries out twice dispersing, in mass ratio absolute ethyl alcohol:
γ-Ce2S3Toner=500~600: 1~8, it is 9.0~13.0 that solution ph is adjusted after being dispersed with stirring uniformly, and it is outstanding that toner is made
Supernatant liquid.
Further, in step (3) of the present invention the dosage of dispersant be primary package presoma powder 5~
15wt%；Package presoma powder primary in mass ratio: absolute ethyl alcohol: deionized water=1~8: 75~250: 200~800, it adjusts
It is 9.0~13.0 to save solution ph；The silicon source solution is according to mass ratio Si4+Silicon source: volume ethanol=1g: 5~8ml is pressed.
In said program, dispersant of the present invention is cetyl trimethylammonium bromide (CTAB), polyvinylpyrrolidine
Ketone (PVP) or polyethylene glycol (PEG)；Zirconium source liquid is that propyl alcohol zirconium, butanol zirconium, zirconium sulfate aqueous solution, zirconium oxychloride are water-soluble
Liquid or acetic acid zirconium；The Si4+Silicon source is ethyl orthosilicate (TEOS), sodium metasilicate or Ludox.
In said program, nonoxidizing atmosphere is according to volume ratio hydrogen in step (4) of the present invention: argon gas=1: 5~
10 mixed atmosphere, calcination temperature are 600~1100 DEG C.Further, calcination processing, institute are carried out using double layer aluminium oxide crucible
It states its lower layer of crucible and places secondary capsulation presoma powder, aerobic substance is placed on upper layer, such as cerium sulphide toner raw material；
Product made from preparation method of the present invention using above-mentioned compound coated red pigment cerium sulphide, by γ-Ce2S3
Toner and the zirconium oxide/silica compound coating layer transparent shell for being wrapped in its surface are constituted, and the compound coating layer is transparent
The average thickness of shell is 30~80nm.
The invention has the advantages that：
(1) present invention improves effective package to cerium sulphide colorant surface by the compound package of fractional hydrolysis-, reacts
Easily controllable, preparation process is reliable and stable, is calcined in conjunction with nonoxidizing atmosphere, effectively increases zirconium oxide/silica compound coating
The consistency of layer.
(2) zirconium oxide of the present invention/silica compound coating layer is fine and close to the package of cerium sulphide toner particle, compact, substantially
Red appearance is still presented at a temperature of 550 DEG C in the Sprouting resistance and high-temperature oxidation resistance for improving cerium sulphide colorant, greatly expands
Its application field.
(3) preparation is simple by the present invention, and obtained product stability is strong, is suitable for industrialization promotion.
Description of the drawings
Below in conjunction with embodiment and attached 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
For the picture of different zones).
Specific implementation mode
Embodiment one：
A kind of preparation method of compound coated red pigment cerium sulphide of the present embodiment, its step are as follows：
(1) a hydrolysis material solution is prepared
Toner suspension：By 0.5g γ-Ce2S3Toner adds with 0.05g dispersants cetyl trimethylammonium bromide (CTAB)
Enter into 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, is aged under magnetic agitation for 24 hours, centrifuge washing once removes
Extra dispersant and impurity and obtain pretreatment colorant；Then pretreatment colorant is added to 75ml absolute ethyl alcohols, magnetic again
Power, which is stirred and is ultrasonically treated, is dispersed with stirring the uniformly rear sodium hydrate regulator solution pH value that 1mol/L is added to carry out twice dispersing
It is 12, and toner suspension is made；
Zirconium source liquid：Using 1ml butanol zirconiums as zirconium source solution；
Hydrolyze auxiliary agent：0.55g anhydrous sodium acetates are dissolved in 5ml deionized waters and hydrolysis auxiliary agent is made；
(2) primary package presoma powder is prepared
Above-mentioned zirconium source liquid is uniformly mixed with toner suspension, ultrasonic disperse 5min and obtain the suspension of toner containing zirconium；It adopts
It is added dropwise in the suspension of toner containing zirconium with the speed of 0.025ml/min by auxiliary agent is hydrolyzed with peristaltic pump, in 30 DEG C of hydrolysis temperatures, slowly
Hydrolysis 2h under fast magnetic agitation, reaction product centrifuge washing obtain once wrapping up presoma in 95 DEG C of baking ovens after drying
Powder；
(3) secondary hydrolysis material solution is prepared
Primary package precursor pulp suspension：0.5g is once wrapped up to presoma powder and 0.05g dispersant hexadecanes
Base trimethylammonium bromide (CTAB) is added in 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, and magnetic agitation simultaneously surpasses
Sound disperses 5min, and the ammonium hydroxide adjusting solution ph for being added 6% is 10.5, and primary package precursor pulp suspension is made；
Silicon source solution：0.6g ethyl orthosilicates are dissolved in 3.5ml absolute ethyl alcohols, silicon source solution is made；
(4) secondary capsulation presoma powder is prepared
Use peristaltic pump that above-mentioned silicon source solution is added dropwise to primary package presoma powder suspension with the speed of 0.1ml/min
In liquid, the hydrolysis 6h in 50 DEG C of hydrolysis temperatures, at a slow speed under magnetic agitation, reaction product centrifuge washing is done 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 powder is placed by lower layer, and upper layer is laid with one layer of vulcanization
Cerium raw material is to consume extra oxygen；Using the mixed atmosphere of the ︰ 8 of volume ratio Qing Qi ︰ argon gas=1 as nonoxidizing atmosphere, by room temperature
~700 DEG C, heating rate is that 5 DEG C/min is further continued for being warming up to 1000 DEG C with 5 DEG C/min and keeps the temperature 2h, so after keeping the temperature 30min
Cooled to room temperature after being cooled to 700 DEG C afterwards with the speed of 5 DEG C/min is obtained with zirconium oxide/silica compound coating
The fine and close compound coated red pigment cerium sulphide of layer, package.
As shown in Figure 1, there is zirconium oxide/silica compound coating layer, wrap up the compound of densification prepared by the present embodiment
Coated red pigment cerium sulphide has dense uniform, transparent clad shell, clad shell on cerium sulphide colorant surface
Average thickness be 60nm.
Embodiment two：
A kind of preparation method of compound coated red pigment cerium sulphide of the present embodiment, its step are as follows：
(1) a hydrolysis material solution is prepared
Toner suspension：By 0.5g γ-Ce2S3Toner adds with 0.05g dispersants cetyl trimethylammonium bromide (CTAB)
Enter into 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, is aged under magnetic agitation for 24 hours, centrifuge washing once removes
Extra dispersant and impurity and obtain pretreatment colorant；Then pretreatment colorant is added to 75ml absolute ethyl alcohols, magnetic again
Power, which is stirred and is ultrasonically treated, is dispersed with stirring the uniformly rear sodium hydrate regulator solution pH value that 1mol/L is added to carry out twice dispersing
It is 12.5, and toner suspension is made；
Zirconium source liquid：Using 1ml butanol zirconiums as zirconium source solution；
Hydrolyze auxiliary agent：The acetum that compound concentration is 2mol/ is as hydrolysis auxiliary agent；
(2) primary package presoma powder is prepared
Above-mentioned zirconium source liquid is uniformly mixed with toner suspension, ultrasonic disperse 5min and obtain the suspension of toner containing zirconium；It adopts
With peristaltic pump with the speed of 0.02ml/min by 2ml hydrolysis auxiliary agent be added dropwise in the suspension of toner containing zirconium, 45 DEG C of hydrolysis temperatures,
Hydrolysis 3h under magnetic agitation at a slow speed, reaction product centrifuge washing obtain once wrapping up forerunner in 95 DEG C of baking ovens after drying
Body powder；
(3) secondary hydrolysis material solution is prepared
Primary package precursor pulp suspension：0.5g is once wrapped up to presoma powder and 0.075g dispersant hexadecanes
Base trimethylammonium bromide (CTAB) is added in 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, and magnetic agitation simultaneously surpasses
Sound disperses 5min, and the ammonium hydroxide adjusting solution ph for being added 6% is 11, and primary package precursor pulp suspension is made；
Silicon source solution：0.6g ethyl orthosilicates are dissolved in 3.5ml absolute ethyl alcohols, silicon source solution is made；
(4) secondary capsulation presoma powder is prepared
Use peristaltic pump that above-mentioned silicon source solution is added dropwise to primary package presoma powder suspension with the speed of 0.1ml/min
In liquid, the hydrolysis 8h in 60 DEG C of hydrolysis temperatures, at a slow speed under magnetic agitation, reaction product centrifuge washing is done 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 powder is placed by lower layer, and upper layer is laid with one layer of vulcanization
Cerium raw material is to consume extra oxygen；Using the mixed atmosphere of the ︰ 8 of volume ratio Qing Qi ︰ argon gas=1 as nonoxidizing atmosphere, by room temperature
~700 DEG C, heating rate is that 5 DEG C/min is further continued for being warming up to 1000 DEG C with 5 DEG C/min and keeps the temperature 2h, so after keeping the temperature 30min
Cooled to room temperature after being cooled to 700 DEG C afterwards with the speed of 5 DEG C/min is obtained with zirconium oxide/silica compound coating
The fine and close compound coated red pigment cerium sulphide of layer, package.
Embodiment three：
A kind of preparation method of compound coated red pigment cerium sulphide of the present embodiment, its step are as follows：
(1) a hydrolysis material solution is prepared
Toner suspension：By 0.3g γ-Ce2S3Toner and 0.045g dispersants cetyl trimethylammonium bromide (CTAB)
It is added in 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, is aged under magnetic agitation for 24 hours, centrifuge washing once removes
It removes extra dispersant and impurity and obtains pretreatment colorant；Then pretreatment colorant is added to 75ml absolute ethyl alcohols again,
Magnetic agitation is simultaneously ultrasonically treated the sodium hydrate regulator solution pH that uniformly rear addition 1mol/L is dispersed with stirring to carry out twice dispersing
Value is 12, and toner suspension is made；
Zirconium source liquid：Using 1ml butanol zirconiums as zirconium source solution；
Hydrolyze auxiliary agent：0.52g ammonium acetates are dissolved in 2ml deionized waters and hydrolysis auxiliary agent is made；
(2) primary package presoma powder is prepared
Above-mentioned zirconium source liquid is uniformly mixed with toner suspension, ultrasonic disperse 5min and obtain the suspension of toner containing zirconium；It adopts
It is added dropwise in the suspension of toner containing zirconium with the speed of 0.025ml/min by auxiliary agent is hydrolyzed with peristaltic pump, in 50 DEG C of hydrolysis temperatures, slowly
Hydrolysis 2.5h under fast magnetic agitation, reaction product centrifuge washing obtain once wrapping up forerunner in 95 DEG C of baking ovens after drying
Body powder；
(3) secondary hydrolysis material solution is prepared
Primary package precursor pulp suspension：0.3g is once wrapped up to presoma powder and 0.045g dispersant hexadecanes
Base trimethylammonium bromide (CTAB) is added in 25ml absolute ethyl alcohols and the mixed solution of 50ml deionized waters, and magnetic agitation simultaneously surpasses
Sound disperses 5min, and the ammonium hydroxide adjusting solution ph for being added 6% is 10.5, and primary package precursor pulp suspension is made；
Silicon source solution：0.6g ethyl orthosilicates are dissolved in 3.5ml absolute ethyl alcohols, silicon source solution is made；
(4) secondary capsulation presoma powder is prepared
It uses peristaltic pump that above-mentioned silicon source solution is added dropwise to primary package presoma powder with the speed of 0.15ml/min to hang
In supernatant liquid, the hydrolysis 12h in 50 DEG C of hydrolysis temperatures, at a slow speed under magnetic agitation, reaction product centrifuge washing, in 95 DEG C of baking ovens
Secondary capsulation presoma powder is obtained after drying；
(5) calcination processing of secondary capsulation presoma powder
Using double layer aluminium oxide crucible, above-mentioned secondary capsulation forerunner powder is placed by lower layer, and upper layer is laid with one layer of vulcanization
Cerium raw material is to consume extra oxygen；Using the mixed atmosphere of the ︰ 8 of volume ratio Qing Qi ︰ argon gas=1 as nonoxidizing atmosphere, by room temperature
~700 DEG C, heating rate is that 5 DEG C/min is further continued for being warming up to 1000 DEG C with 5 DEG C/min and keeps the temperature 2h, so after keeping the temperature 30min
Cooled to room temperature after being cooled to 700 DEG C afterwards with the speed of 5 DEG C/min is obtained with zirconium oxide/silica compound coating
The fine and close compound coated red pigment cerium sulphide of layer, package.
Compound coated red pigment cerium sulphide obtained by various embodiments of the present invention, chromatic value are as shown in table 1.
The chromatic value of the compound coated red pigment cerium sulphide of 1 various embodiments of the present invention of table
| 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 |
As a comparison case with the commercial cerium sulphide colorant that does not wrap up, the compound coated sulphur obtained by the embodiment of the present invention one
Change cerium red pigment, the chromatic value in air atmosphere under different calcination temperatures is as shown in table 2.
The chromatic value of 2 embodiment of the present invention one of table and comparative example in air atmosphere under different calcination temperatures
Claims (6)
1. a kind of preparation method of compound coated red pigment cerium sulphide, it is characterised in that include the following steps：
(1) a hydrolysis material solution is prepared
Toner suspension：It is carried out by the way of twice dispersing, first by γ-Ce2S3Toner and dispersant cetyl trimethyl
Ammonium bromide, which is added in absolute ethyl alcohol and the mixed solution of deionized water, once to be disperseed, γ-Ce in mass ratio2S3Toner: nothing
Water-ethanol: deionized water=1~8: 75~250: 200~800, the dosage of the dispersant is γ-Ce2S3The 5 of toner~
15wt%, after stirring ageing, centrifugal treating obtains pretreatment colorant to remove extra dispersant and impurity；It then will be described
Pretreatment colorant, which is added to again in absolute ethyl alcohol, carries out twice dispersing, in mass ratio absolute ethyl alcohol: γ-Ce2S3Toner=500
~600: 1~8, it is 9.0~13.0 that solution ph is adjusted after being dispersed with stirring uniformly, and toner suspension is made；
Zirconium source liquid：Containing Zr4+Liquid flux；
Hydrolyze auxiliary agent：Acetic acid, sodium hydroxide, sodium acetate, potassium hydroxide or ammonium acetate are dissolved in deionized water and concentration is made
For the hydrolysis auxiliary agent of 1~4mol/L；
(2) primary package presoma powder is prepared
According to molar ratio Zr4+∶γ-Ce2S3=1~10: 1~2, zirconium source liquid is uniformly mixed with toner suspension and is obtained
The suspension of toner containing zirconium；By volume of water enzymolysis auxiliary agent: pressing quality γ-Ce2S3Toner=1~10mL: 0.1~1g, by the hydrolysis
Auxiliary agent is added to stirring in the suspension of toner containing zirconium with the speed of 0.02~0.2mL/min and reaction is hydrolyzed, and reaction temperature is
20~50 DEG C, the reaction time is 1~6h；It obtains once wrapping up presoma powder after reaction product cleaning, drying；
(3) secondary hydrolysis material solution is prepared
Primary package precursor pulp suspension：To once wrap up presoma powder, dispersant cetyl trimethylammonium bromide,
Absolute ethyl alcohol, deionized water are blended and evenly dispersed, adjust solution ph in alkalinity, primary package presoma powder suspension is made
Liquid；
Silicon source solution：By Si4+Silicon source is mixed to prepare silicon source solution with ethyl alcohol；
(4) secondary capsulation presoma powder is prepared
According to molar ratio Si4+∶γ-Ce2S3=1~3: 1~2, by the silicon source solution with the speed of 0.02~0.15mL/min
It is added to stirring in primary package precursor pulp suspension and reaction is hydrolyzed, reaction temperature is 30~90 DEG C, the reaction time
For 2~16h；Secondary capsulation presoma powder is obtained after reaction product cleaning, drying；
(5) calcination processing of secondary capsulation presoma powder
By the secondary capsulation presoma powder under nonoxidizing atmosphere calcination processing, obtain multiple with zirconium oxide/silica
Close the fine and close compound coated red pigment cerium sulphide of clad, package.
2. the preparation method of compound coated red pigment cerium sulphide according to claim 1, it is characterised in that：The step
Suddenly the dosage of dispersant is the primary 5~15wt% for wrapping up presoma powder in (3)；Presoma powder is once wrapped up in mass ratio:
Absolute ethyl alcohol: deionized water=1~8: 75~250: 200~800, it is 9.0~13.0 to adjust solution ph；The silicon source solution
According to mass ratio Si4+Silicon source: volume ethanol=1g: 5~8mL is pressed.
3. the preparation method of compound coated red pigment cerium sulphide according to claim 1 or 2, it is characterised in that：Institute
It is propyl alcohol zirconium, butanol zirconium, zirconium sulfate aqueous solution, zirconium oxychloride aqueous solution or acetic acid zirconium to state zirconium source liquid；The Si4+Silicon source is just
Silester, sodium metasilicate or Ludox.
4. the preparation method of compound coated red pigment cerium sulphide according to claim 1, it is characterised in that：The step
Suddenly nonoxidizing atmosphere is according to volume ratio hydrogen in (5): argon gas=1: 5~10 mixed atmosphere, calcination temperature are 600~1100
℃。
5. the preparation method of compound coated red pigment cerium sulphide according to claim 4, it is characterised in that：The step
Suddenly (5) carry out calcination processing using double layer aluminium oxide crucible, and secondary capsulation presoma powder is placed by its lower layer of the crucible, thereon
Layer places aerobic substance.
6. using product made from one of the claim 1-5 preparation methods of the compound coated red pigment cerium sulphide,
It is characterized in that：By γ-Ce2S3Toner and the zirconium oxide/silica compound coating layer transparent shell for being wrapped in its surface are constituted,
The average thickness of the compound coating layer transparent shell is 30~80nm.
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| CN106928752B (en) * | 2017-02-28 | 2018-05-04 | 景德镇陶瓷大学 | A kind of zirconium silicate using zirconium carbonate ammonium as zirconium source wraps up the preparation method of ceramic pigment |
| CN107758720B (en) * | 2017-10-25 | 2019-04-30 | 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 |
| CN108219536B (en) * | 2017-12-12 | 2020-07-10 | 景德镇陶瓷大学 | Alumina-coated gamma-Ce2S3Preparation method of red pigment |
| 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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