CN106928752A - A kind of preparation method of zirconium silicate parcel ceramic pigment with zirconium carbonate ammonium as zirconium source and its obtained product - Google Patents
A kind of preparation method of zirconium silicate parcel ceramic pigment with zirconium carbonate ammonium as zirconium source and its obtained product Download PDFInfo
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- CN106928752A CN106928752A CN201710114698.3A CN201710114698A CN106928752A CN 106928752 A CN106928752 A CN 106928752A CN 201710114698 A CN201710114698 A CN 201710114698A CN 106928752 A CN106928752 A CN 106928752A
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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
- C09C1/0012—Pigments for ceramics containing zirconium and silicon
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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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Abstract
The invention discloses the preparation method that a kind of zirconium silicate with zirconium carbonate ammonium as zirconium source wraps up ceramic pigment, stir to form stable suspension with zirconium carbonate ammonium solution after colouring agent powder is disperseed first, deposited by reacting to be formed on coloring agent particle surface, so as to obtain zirconium oxide wrappage；Then zirconium oxide wrappage addition silicon source solution is well mixed, regulation pH value is precipitated, and ceramic pigment presoma is obtained through dried process；The ceramic pigment presoma is through calcining and removes the colouring agent not wrapped up, that is, obtain zirconium silicate parcel ceramic pigment powder.Additionally, also disclosing using product obtained in above-mentioned preparation method.The present invention can avoid the destruction caused to ceramic pigment, and form encapsulation ratio high, the occlusion pigment with core shell structure, efficiently solve the problems, such as zirconium silicate parcel ceramic pigment encapsulation ratio high and colouring agent account for pigment proportion it is low between contradict, so as to effectively increase occlusion pigment in color depth, reduce addition when using.
Description
Technical field
The present invention relates to ceramic pigment technical field, more particularly to a kind of coated ceramic pigment preparation method and its system
The product for obtaining.
Background technology
Zirconium silicate ZrSiO4With fusing point is high, refractive index big, stable chemical nature, high temperature resistance melt attack the features such as, mesh
It is preceding to have turned into the first-selected wrapper material of parcel ceramic pigment, to cadmium sulfoselenide, carbon black, Fe2O3Deng the parcel of toner, with good
Good application effect.However, prior art zirconium silicate parcel ceramic pigment generally existing colouring agent encapsulation ratio is low, colouring agent accounts for color
The low problem of material ratio, for example, during zirconium silicate parcel carbon black colorant is prepared, using being easy to the industrialized precipitation method
When, due to the characteristic that carbon black is not hydrophilic so that the encapsulation ratio of the parcel carbon black colorant prepared is not wrapped up far below 8~11%
Carbon black can only be calcined by secondary oxidation and remove, and mass ratio shared by carbon black only about 5% in colorant finished product；Due to encapsulation ratio and
It is low that colouring agent accounts for pigment proportion, and zirconium silicate parcel carbon black is typically only capable to show as grey (colorant lightness L*>30).For another example, at present
The zirconium silicate parcel cadmium sulfoselenide prepared using the precipitation method in production, Cd (S1-xSex) encapsulation ratio it is general in 5~8%, production
When, the cadmium sulfoselenide quality of input accounts for the quality about 40% of ceramic pigment finished product, and otherwise, excessive cadmium sulfoselenide can be because cannot be complete
Wrap up and oxidation Decomposition entirely.Due to Cd (S1-xSex) encapsulation ratio it is general 5~8%, cadmium sulfoselenide matter in such colorant finished product
The quality highest that amount accounts for ceramic pigment finished product only has 3.2%, so as to cause red pigment color partially light.
At present, the preparation technology of zirconium silicate occlusion pigment mainly has two kinds of the precipitation method, sol-gel process, and the precipitation method are main
It is zirconium source with zirconium oxychloride；Sol-gel process is mainly used in laboratory, is zirconium source with zirconium chloride, zirconium oxychloride, alcohol zirconium.Though
Right prior art improves the encapsulation ratio of zirconium silicate and improves using effect by strengthening the mixing of zirconium silicate and toner, but
Remain following technological deficiency：(1) raising of above-mentioned encapsulation ratio is realized by increasing the ratio of zirconium silicate, and this must
So cause colouring agent to be wrapped up by thick silicic acid zirconium layer, significantly reduce colouring agent and account for pigment proportion, so as to have impact on coloring
The colour generation of agent, the color of gained colorant is shallower.In order to obtain certain color depth, it is necessarily required to greatly increase colorant in reality
Consumption in.(2) most of ceramic pigments are metal oxide, with alkaline-resisting acid nonfast characteristic.And with zirconium chloride
Or zirconium oxychloride is zirconium source, either its aqueous solution is still prepared into colloidal sol, in acidity, can be with cadmium sulfoselenide or Fe2O3
Generation chemically reacts and destroys colouring agent, even if zirconium oxychloride and zirconium chloride are prepared into ZrO2Colloidal sol, ZrO2The pH value of colloidal sol
About 3~5, still can be with cadmium sulfoselenide or Fe2O3Chemically react, thus be difficult to synthesize and obtain with nucleocapsid structure
Zirconium silicate wraps up ceramic pigment.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of zirconium silicate bag with zirconium carbonate ammonium as zirconium source
The preparation method of ceramic pigment is wrapped up in, is used as zirconium source in weakly alkaline zirconium carbonate ammonium by using, it is to avoid ceramic pigment is caused brokenly
It is bad, and by the deposition on coloring agent particle surface, encapsulation ratio high, the occlusion pigment with nucleocapsid structure are formed, effectively to solve
Certainly zirconium silicate parcel ceramic pigment encapsulation ratio high and colouring agent account for pigment proportion it is low between the problem that contradicts, so as to effectively improve
Occlusion pigment in color depth, reduction use when addition.Another object of the present invention is to provide using above-mentioned preparation side
Product obtained in method.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of zirconium silicate parcel ceramic pigment with zirconium carbonate ammonium as zirconium source that the present invention is provided, including with
Lower step：
(1) stir to form stable suspension with zirconium carbonate ammonium solution after colouring agent powder is disperseed, in mass ratio
Toner: zirconium oxide=1: 1~4 (zirconium oxide can be obtained by zirconium carbonate ammonium conversion)；The suspension is placed in 40~60 DEG C of baking ovens
2~12h of interior treatment, forms zirconium oxide coated powder suspension, after drying, crushing, obtains zirconium oxide coated powder；
(2) add silicon source solution to be well mixed the zirconium oxide coated powder or zirconium oxide coated powder suspension, press
Quality is than zirconium oxide: silica=1: 0.5~0.75, regulation pH value is precipitated, and ceramic pigment forerunner is obtained through dried process
Body；
(3) mineralizer is added to be well mixed in the ceramic pigment presoma, after carrying out quick burning, removal is not wrapped up
Colouring agent, that is, obtain zirconium silicate parcel ceramic pigment powder.
The present invention using zirconium carbonate ammonium as zirconium source, its pH value be 9~10, in alkalescent, will not with cadmium sulfoselenide or
Fe2O3Chemically react, when temperature is higher than 60 DEG C, meeting fast decoupled generates cotton-shaped zirconium oxide, it is difficult to form fine and close parcel
Layer, therefore using the decomposition rate of relatively low temperature control zirconium carbonate ammonium so that the zirconium oxide for obtaining is decomposed in coloring agent particle
Surface gradually increases to form one layer of fine and close beds of precipitation, and the clad can cover all surface of coloring agent particle.Added again
Enter in silicon source solution, by adjusting pH value, silica clad can be formed on zirconia layer surface.By quick burning, oxidation
Zirconium and silica clad are changed into the zirconium silicate integument of densification, the final zirconium silicate occlusion pigment for obtaining full parcel.
Further, it is more to contribute to control the decomposition of zirconium carbonate ammonium and the thickness of integument, step of the present invention
Suddenly the concentration of zirconium carbonate ammonium solution is 10~30wt% in (1).
In such scheme, the dried process of zirconium oxide coated powder suspension in step (1) of the present invention, using 150
~200 DEG C of baking ovens are carried out, when being lost to massless.
Further, pH value is 7.5~10.0 in step (2) of the present invention.Quick burning system in the step (3)
For：1000~1150 DEG C are warming up to the heating rate of 40~100 DEG C/min, soaking time is 10~60min.
Additionally, mineralizer of the present invention is magnesium chloride, lithium fluoride, sodium fluoride or magnesium fluoride.
Colouring agent powder of the present invention is carbon black, cadmium sulfoselenide or Fe2O3。
Product obtained in the preparation method of ceramic pigment is wrapped up using the above-mentioned zirconium silicate with zirconium carbonate ammonium as zirconium source.
The invention has the advantages that：
(1) present invention is zirconium source with zirconium carbonate ammonium solution, makes its slow decomposition, analyte homogeneous precipitation at a certain temperature
In all surfaces of coloring agent particle, form zirconium oxide occlusion pigment powder/suspension, thus obtain encapsulation ratio high, with core-
The occlusion pigment presoma of shell structure.By controlling concentration and the reaction time of zirconium carbonate ammonium solution, zirconium oxide bag can be controlled
The thickness of covering layer, makes the encapsulation ratio of colouring agent reach 40~85%；Because the ratio of silica and zirconium oxide is certain, oxidation
When the thickness of zirconium layer is smaller with respect to colouring agent particle diameter, the quality shared by zirconium silicate is smaller, therefore, colouring agent/colorant mass ratio
Reached 10~20%, 1 times at least improve than existing occlusion pigment, so as to improve occlusion pigment in color depth, have
Effect solve the problems, such as zirconium silicate parcel ceramic pigment encapsulation ratio high and colouring agent account for pigment proportion it is low between contradict.
(2) the zirconium carbonate ammonium solution that the present invention is used is in alkalescent, will not be reacted with most of ceramic pigments, thus
Preparation method of the present invention is applied widely, with good adaptability.
Brief description of the drawings
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail：
Fig. 1 is the transmission electron microscope photo that the gained zirconium silicate of the embodiment of the present invention three wraps up cadmium sulfoselenide colorant powder.
Specific embodiment
Embodiment one：
A kind of zirconium silicate with zirconium carbonate ammonium as zirconium source of the present embodiment wraps up the preparation method of ceramic pigment, and its step is such as
Under：
(1) by 10g carbon blacks, 0.5g 10wt%PEG-200 solution and 200mL water, strong agitation forms stable suspension,
It is then added to the zirconium carbonate ammonium solution that 200mL concentration is 25wt% and (contains 19wt%ZrO after conversion in solution2) in, stirring is equal
55 DEG C of oven 4h are placed in after even, zirconium oxide coated powder suspension is formed；Through 150 DEG C of baking ovens to after being completely dried, with broken
Broken machine is crushed and obtains zirconium oxide parcel carbon black powder；
(2) add 20g concentration to be well mixed for the Ludox of 30wt% above-mentioned 10g zirconium oxides parcel carbon black powder, make
It is 9 to adjust pH value with weak aqua ammonia, forms gel, and is heated to 150 DEG C to drying, and obtains ceramic pigment presoma；
(3) lithium fluoride that consumption is its 3wt% is added in above-mentioned ceramic pigment presoma, it is uniform by ball milling mixing
Afterwards, 1150 DEG C are warming up to the heating rate of 40 DEG C/min, 20min is incubated under nonoxidizing atmosphere；Then after lowering the temperature with stove,
900 DEG C, calcine 2h in oxidizing atmosphere, to remove the carbon black not wrapped up, that is, obtain zirconium silicate parcel carbonarius feed powder body.
The encapsulation ratio of the zirconium silicate parcel carbonarius feed powder body prepared by the present embodiment is 80%, and carbon black is accounted in colorant finished product
The mass ratio of colorant finished product is 10%, and colourity is：L*=27.54, a*=0.31, b*=-0.21.
Embodiment two：
A kind of zirconium silicate with zirconium carbonate ammonium as zirconium source of the present embodiment wraps up the preparation method of ceramic pigment, with embodiment one
Difference is：
In step (1), zirconium carbonate ammonium solution contains 20wt%ZrO2；The zirconium oxide coated powder suspension for being formed without
Cross dry, pulverization process.
In step (2), it is the silicon of 30wt% that the zirconium oxide coated powder suspension that step (1) is formed adds 100g concentration
Colloidal sol is well mixed.
The encapsulation ratio of the zirconium silicate parcel carbonarius feed powder body prepared by the present embodiment is 85%, and carbon black is accounted in colorant finished product
The mass ratio of colorant finished product is 10.8%, and colourity is：L*=23.81, a*=-0.51, b*=-0.13.
Embodiment three：
A kind of zirconium silicate with zirconium carbonate ammonium as zirconium source of the present embodiment wraps up the preparation method of ceramic pigment, and its step is such as
Under：
(1) by 10g cadmium sulfoselenides (the commercially available cadmium-selenium red colorant not wrapped up), 0.5g PEG-200 solution, 50g water and 50g
Zirconium carbonate ammonium solution (contains 20wt%ZrO in solution2) in, quick stirring forms stable suspension, is placed in 55 DEG C of oven 8h,
Form zirconium oxide coated powder suspension；Through 150 DEG C of baking ovens to after being completely dried, zirconium oxide is obtained after being crushed with disintegrating machine and is wrapped up
Cadmium sulfoselenide powder；
(2) add 20g concentration to be well mixed for the Ludox of 30wt% above-mentioned zirconium oxide parcel cadmium sulfoselenide powder, make
It is 9 to adjust pH value with weak aqua ammonia, forms gel, and microwave drying obtains ceramic pigment presoma；
(3) lithium fluoride that consumption is its 3wt% is added in above-mentioned ceramic pigment presoma, it is uniform by ball milling mixing
Afterwards, 1150 DEG C are warming up to the heating rate of 100 DEG C/min, are incubated 10min；Then take out chilling and obtain initial colorant, by this
Initial colorant soaks 5h using concentrated nitric acid, after cleaning up, reuses 10wt% sodium hydroxide solution immersion treatment 4h, and cleaning is extremely
PH=7, that is, obtain zirconium silicate parcel cadmium sulfoselenide colorant powder.
The encapsulation ratio of the zirconium silicate parcel cadmium sulfoselenide colorant powder prepared by the present embodiment is 40%, sulphur in colorant finished product
The mass ratio that cadmium selenide accounts for colorant finished product is 20%.As shown in figure 1, being zirconium silicate around cadmium sulfoselenide particle (black portions)
Integument.Soaked using concentrated nitric acid, produced without obvious bubble, the colourity of zirconium silicate parcel cadmium sulfoselenide colorant powder is：L*=
45.30, a*=21.24, b*=18.25.
Claims (8)
1. a kind of zirconium silicate with zirconium carbonate ammonium as zirconium source wraps up the preparation method of ceramic pigment, it is characterised in that including following step
Suddenly：
(1) stir to form stable suspension with zirconium carbonate ammonium solution after colouring agent powder is disperseed, in mass ratio colouring agent:
Zirconium oxide=1: 1~4；The suspension is placed in 2~12h for the treatment of in 40~60 DEG C of baking ovens, zirconium oxide coated powder is formed and is hanged
Supernatant liquid, after drying, crushing, obtains zirconium oxide coated powder；
(2) silicon source solution is added to be well mixed the zirconium oxide coated powder or zirconium oxide coated powder suspension, by quality
Than zirconium oxide: silica=1: 0.5~0.75, regulation pH value is precipitated, and ceramic pigment presoma is obtained through dried process；
(3) mineralizer is added to be well mixed in the ceramic pigment presoma, after carrying out quick burning, what removal was not wrapped up
Toner, that is, obtain zirconium silicate parcel ceramic pigment powder.
2. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：The concentration of zirconium carbonate ammonium solution is 10~30wt% in the step (1).
3. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：The dried process of zirconium oxide coated powder suspension, is carried out, extremely using 150~200 DEG C of baking ovens in the step (1)
Untill when massless are lost.
4. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：PH value is 7.5~10.0 in the step (2).
5. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：Quick burning system is in the step (3)：1000~1150 are warming up to the heating rate of 40~100 DEG C/min
DEG C, soaking time is 10~60min.
6. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：The mineralizer is magnesium chloride, lithium fluoride, sodium fluoride or magnesium fluoride.
7. the zirconium silicate with zirconium carbonate ammonium as zirconium source according to claim 1 wraps up the preparation method of ceramic pigment, and it is special
Levy and be：The colouring agent powder is carbon black, cadmium sulfoselenide or Fe2O3。
8. the preparation method system of ceramic pigment is wrapped up using one of the claim 1-7 zirconium silicates with zirconium carbonate ammonium as zirconium source
The product for obtaining.
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| CN107459369A (en) * | 2017-09-07 | 2017-12-12 | 景德镇陶瓷大学 | One kind prepares ZrSiO using non-hydrolytic sol-gel technique in SiC substrates4The method of film |
| CN107500807A (en) * | 2017-09-30 | 2017-12-22 | 江西金环颜料有限公司 | A kind of preparation method of high temperature resistant green ceramic pigment |
| CN108084796A (en) * | 2017-12-15 | 2018-05-29 | 佛山市扬子颜料有限公司 | A kind of new package carbon black ceramics marking ink and preparation method thereof |
| CN108219538A (en) * | 2018-02-26 | 2018-06-29 | 山东好白陶瓷原料有限公司 | A kind of preparation method of ultrawhite zirconium silicate |
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| CN114182111A (en) * | 2022-01-05 | 2022-03-15 | 东北大学 | Method for extracting zirconium oxide from zirconium silicate |
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| CN107500807A (en) * | 2017-09-30 | 2017-12-22 | 江西金环颜料有限公司 | A kind of preparation method of high temperature resistant green ceramic pigment |
| CN108084796A (en) * | 2017-12-15 | 2018-05-29 | 佛山市扬子颜料有限公司 | A kind of new package carbon black ceramics marking ink and preparation method thereof |
| CN108219538A (en) * | 2018-02-26 | 2018-06-29 | 山东好白陶瓷原料有限公司 | A kind of preparation method of ultrawhite zirconium silicate |
| CN109135337A (en) * | 2018-07-18 | 2019-01-04 | 佛山市三水金鹰无机材料有限公司 | A kind of preparation method of Portoro ceramic ink jet colorant |
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| CN110655807A (en) * | 2019-09-29 | 2020-01-07 | 江西金环颜料有限公司 | Preparation method of zirconium silicate coated iron oxide red for ceramic ink-jet printing |
| CN110655807B (en) * | 2019-09-29 | 2021-06-15 | 江西金环颜料有限公司 | Preparation method of zirconium silicate coated iron oxide red for ceramic ink-jet printing |
| CN112960906A (en) * | 2021-04-13 | 2021-06-15 | 刘永广 | Lead-free environment-friendly ceramic glaze and preparation method thereof |
| CN113479895A (en) * | 2021-07-05 | 2021-10-08 | 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 |
| CN114182111A (en) * | 2022-01-05 | 2022-03-15 | 东北大学 | Method for extracting zirconium oxide from zirconium silicate |
| CN114182111B (en) * | 2022-01-05 | 2022-09-27 | 东北大学 | Method for extracting zirconium oxide from zirconium silicate |
| CN115286244A (en) * | 2022-07-15 | 2022-11-04 | 广州铁路职业技术学院（广州铁路机械学校） | Special gray digital overglaze for ceramic large plate, synthesis method and application |
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