CN108084795A - A kind of ceramic ink zaffre and preparation method thereof - Google Patents
A kind of ceramic ink zaffre and preparation method thereof Download PDFInfo
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- CN108084795A CN108084795A CN201711434201.2A CN201711434201A CN108084795A CN 108084795 A CN108084795 A CN 108084795A CN 201711434201 A CN201711434201 A CN 201711434201A CN 108084795 A CN108084795 A CN 108084795A
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- zaffre
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
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- Wood Science & Technology (AREA)
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Abstract
The invention discloses a kind of preparation methods of ceramic ink zaffre, include the following steps：S1. cobalt source, silicon source and silicon source are weighed；S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed；S4. calcine：Beat powder after raw material calcined at 1130 DEG C ~ 1200 DEG C 2 ~ 3 it is small when；S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.The present invention is synthesized by solid reaction process with CoO Al after mixing cobalt source, silicon source, silicon source raw material2O3Spinelle and 2 CoO SiO2Mixed crystal based on olivine, Al in formula2O3And SiO2Eutectic point can be formed in glaze, it so can be to avoid negative effect of the colorant to glaze paint；Simultaneously inventor it was unexpectedly found that, the colorant of preparation is compared to than CoO Al2O3Spinelle, 2 CoO SiO2The colorant that olivine is prepared separately, colour generation ability significantly improves in glaze.
Description
Technical field
The present invention relates to ceramic pigment technical field, more particularly to a kind of ceramic ink zaffre and its preparation
Method.
Background technology
After the decoration of ceramic experienced screen printing, roller printing, inkjet printing has been started again in recent years
Climax.Inkjet printing technology has been referred to as the third time revolution of China's ceramic wall and floor bricks printing technique, more and more domestic potteries
Porcelain enterprise has an optimistic view of this developing direction.Ink-jet printer has many unrivaled advantages compared with screen printing and roller printing：
It due to being contactless decoration, can be decorated in arbitrary convex-concave surface, product therefore more personalized, true to nature, fine and smooth,
More rich texture variations.Simultaneously because air brushing technology need not web plate processed, not only save the time, but improve efficiency, therefore, in market
It is upper extremely welcome, and market development space is very big.
Ceramic ink is usually by inorganic non-metallic material（Colorant, glaze, functional material）, solvent, dispersant, bonding agent,
Surfactant and other auxiliary materials are formed.Inorganic non-metallic material（Colorant, glaze, functional material）It is the core substance of ink,
Its grain graininess should be less than 1 μm, and particle size distribution is relatively narrow, have preferable dispersiveness and stability, by other objects such as solvent
The influence of matter is smaller.
Blueness is one of three big main primary colours, many Neutral colour and tertiary colour lack its can not, thus to become the five colours in riotous profusion for blueness
The chief component of confused color.Zaffre is important spinel-type blueness colorant, alternatively referred to as aluminic acid cobalt blue.It is most simple
Chemical formula be CoO Al2O3, compared with other blue colorants, there is excellent light resistance, weatherability, heat resistance, resistance toization
The performances such as corrosivity, nontoxic are learned, therefore are widely used in high-temperature resistant coating, ceramics, enamel, glass, coloring plastic.But with
CoO•Al2O3Alumina content accounts for 60wt% in zaffre based on spinelle, since the fusing point of aluminium oxide is up to 2045 DEG C,
When the ceramic ink that this kind of zaffre is prepared into is sprayed in glaze paint, the excessive aluminium oxide of glaze paint Local enrichment causes glaze paint to melt
Melt temperature raising, glaze paint is caused out-of-flatness, wrinkling occur, influences the beauty of glaze paint.
The content of the invention
The defects of in order to make up prior art, the present invention provide a kind of ceramic ink zaffre and preparation method thereof.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of preparation method of ceramic ink zaffre, includes the following steps：
S1. raw material is weighed：Molar ratio by Co: Al: Si is (2 ~ 4):(2~2.5):(3 ~ 5) weigh cobalt source, silicon source and silicon respectively
Source；
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：Beat powder after raw material calcined at 1130 DEG C ~ 1200 DEG C 2 ~ 3 it is small when；
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
Further, the cobalt source is cobalt oxide, cobalt carbonate or cobalt hydroxide.
Further, source of aluminium is aluminium hydroxide or calcined alumina.
Further, the silicon source is quartz.
Further, the cobalt source is machined to fineness D100 no more than 10 μm through airflow mill.
Further, source of aluminium is machined to fineness D100 no more than 5 μm through airflow mill.
Further, the silicon source is machined to fineness D100 no more than 10 μm through airflow mill.
Further, in step S1, the raw material further includes magnesia and/or zinc oxide.
Further, in step S1, the raw material does not include mineralizer.
The present invention also provides the ceramic ink zaffres being prepared by above-mentioned preparation method.
The present invention has the advantages that：
The present invention is synthesized by solid reaction process with CoO Al after mixing cobalt source, silicon source, silicon source raw material2O3Spinelle and 2
CoO•SiO2Mixed crystal based on olivine, Al in formula2O3And SiO2Eutectic point can be formed in glaze, it so can be with
Avoid negative effect of the colorant to glaze paint；Simultaneously inventor it was unexpectedly found that, in CoO Al2O3Draw on the basis of spinelle
Enter SiO2, form CoO Al2O3Spinelle and 2CoO SiO2The mixed structure of olivine, the colorant of preparation is compared to than CoO
Al2O3Spinelle, 2 CoO SiO2The colorant that olivine is prepared separately, colour generation ability significantly improves in glaze.
The present invention prepares zaffre using high-temperature calcination solid reaction process, and simple production process, production cost is relatively low, more
It is appropriate to ceramic industry.
Zaffre color development saturation degree prepared by the present invention is high, disclosure satisfy that the requirement of ceramic ink.
The hardness of zaffre prepared by the present invention is low, is conducive to be ground into the smaller powder of grain size；Ore deposit is free of in colorant
Agent need not wash.
Specific embodiment
A kind of preparation method of ceramic ink zaffre, includes the following steps：
S1. raw material is weighed：The raw material includes cobalt source, silicon source and silicon source.
In the present invention, Co: Al: Si molar ratio is (2 ~ 4) in the raw material:(2~2.5):(3~5).Rationally control of the invention
The ratio of cobalt source processed, silicon source and silicon source, makes aluminium and silicon suitably excessive, and the product appearance being prepared is in vivid blue, Bu Huibian
It is black.
In the present invention, the cobalt source is preferably cobalt oxide, cobalt carbonate or cobalt hydroxide, but not limited to this.The cobalt source
Fineness D100 is machined to no more than 10 μm through airflow mill in advance, it is preferable that is machined to fineness D100 less than 7 μm.
In the present invention, source of aluminium is preferably aluminium hydroxide or calcined alumina, but not limited to this.Source of aluminium is advance
Fineness D100 is machined to no more than 5 μm through airflow mill, it is preferable that is machined to fineness D100 less than 3 μm.
In the present invention, the silicon source is preferably quartz, but not limited to this.The silicon source is machined in advance through airflow mill
Fineness D100 is no more than 10 μm, it is preferable that is machined to fineness D100 less than 8 microns.
The fineness D100 of raw material used in common colorant is 40 μm ~ 60 μm, and the fineness D100 of the colorant prepared is 25 μm
~40μm.Since ceramic ink needs colorant being ground to fineness D100≤1 μm, colorant can be constantly destroyed in process of lapping
Structure, the raw material that inside fails to participate in reaction will expose the original colorant ingredient of dilution, this will influence to reduce color
Expect the colour generation ability in glaze.Reaction rate constant K values are shown according to solid reaction process poplar Dare, golden Stringer dynamics
Inverse ratio and particle radius square；Particle size is smaller, and reaction system specific surface area is bigger, and reaction interface and diffusion interface are also corresponding
Increase.In the present invention, fineness is controlled with hand since raw material, since the initial particle of done colorant is smaller, is ground in ink
Structure is destroyed few during mill, so as to improve colour generation ability.
It should be noted that the raw material of the present invention does not include mineralizer.
Mineralizer can promote the reaction of colorant group, reduce the temperature of colorant synthesis, existing zaffre is generally all
Using boric acid or borax as mineralizer, and the electrical conductivity for being prepared into ceramic ink requirement colorant is as low as possible, due to mineralizer
Belong to soluble-salt substance, the electrical conductivity of colorant can be increased substantially containing mineralizing components, this requires colorant needs to wash
Ceramic ink can be just used to prepare；And the existing zaffre without using mineralizer its calcining heat is concentrated mainly on 1250-
Between 1300 DEG C, the excessively high quality that can reduce colorant of calcining heat.The present invention is in CoO Al2O3It is introduced on the basis of spinelle
SiO2 does not use mineralizer, need not wash, and calcining heat is reduced to 1130 DEG C ~ 1200 DEG C, and the quality of zaffre is good.
As a further improvement, the raw material further includes magnesia and/or zinc oxide, Co: Al: Si in raw material：Mg/Zn's
Molar ratio is (2 ~ 4):(2~2.5):(3~5) : (0~5).
A certain amount of magnesia and/or zinc oxide are added in the present invention, color development can be made more bright-coloured, while it can take
For part cobalt source, production cost is reduced.
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：The raw material beaten after powder is calcined；
In the present invention, the temperature of calcining is 1130 DEG C ~ 1200 DEG C, when the time of calcining is 2 ~ 3 small；It is highly preferred that the temperature of calcining
It spends for 1150 DEG C ~ 1180 DEG C.
Mineralizer is not contained in the formula of the present invention, liquid phase is not formed after calcining, and calcining heat is low in the present invention so that
The zaffre hardness arrived is low, is conducive to be ground into the smaller powder of grain size.
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
The present invention is synthesized by solid reaction process with CoO Al after mixing cobalt source, silicon source, silicon source raw material2O3Spinelle and 2
CoO• Al2O3Mixed crystal based on olivine, Al in formula2O3And SiO2Eutectic point can be formed in glaze, it so can be with
Avoid negative effect of the colorant to glaze paint；Simultaneously inventor it was unexpectedly found that, in CoO Al2O3Draw on the basis of spinelle
Enter SiO2, form CoO Al2O3Spinelle and 2 CoO SiO2The mixed structure of olivine, the colorant of preparation compared to than
CoO•Al2O3Spinelle, 2 CoO SiO2The colorant that olivine is prepared separately, colour generation ability significantly improves in glaze.
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of preparation method of ceramic ink zaffre, includes the following steps：
S1. raw material is weighed：The raw material is cobalt source, silicon source and silicon source, and Co: Al: Si molar ratio is 3 in raw material:2.2:4；
The cobalt source is cobalt oxide, and the cobalt source is machined to fineness D100 less than 7 μm through airflow mill in advance；Source of aluminium is hydrogen
Aluminium oxide, source of aluminium are machined to fineness D100 less than 3 μm through airflow mill in advance；The silicon source is quartz, and the silicon source is pre-
First fineness D100 is machined to less than 8 microns through airflow mill；
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：Beat powder after raw material calcined at 1180 DEG C 2 ~ 3 it is small when；
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
Embodiment 2
A kind of preparation method of ceramic ink zaffre, includes the following steps：
S1. raw material is weighed：The raw material is cobalt source, silicon source and silicon source, and Co: Al: Si molar ratio is 2 in raw material: 2.5: 5；
The cobalt source is cobalt carbonate, and the cobalt source is machined to fineness D100 less than 7 μm through airflow mill in advance；Source of aluminium is to forge
Aluminium oxide is burnt, source of aluminium is machined to fineness D100 less than 3 μm through airflow mill in advance；The silicon source is quartzy, the silicon source
Fineness D100 is machined to less than 8 microns through airflow mill in advance；
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：Beat powder after raw material calcined at 1130 DEG C 2 ~ 3 it is small when；
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
Embodiment 3
A kind of preparation method of ceramic ink zaffre, includes the following steps：
S1. raw material is weighed：The raw material is cobalt source, silicon source, silicon source and magnesia, Co: Al: Si in raw material：The molar ratio of Mg is
4:2:5:2；
The cobalt source is cobalt hydroxide, and the cobalt source is machined to fineness D100 less than 7 μm through airflow mill in advance；Source of aluminium is
Aluminium hydroxide, source of aluminium are machined to fineness D100 less than 3 μm through airflow mill in advance；The silicon source is quartzy, the silicon source
Fineness D100 is machined to less than 8 microns through airflow mill in advance；
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：Beat powder after raw material calcined at 1150 DEG C 2 ~ 3 it is small when；
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
Embodiment described above only expresses embodiments of the present invention, and description is more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (10)
1. a kind of preparation method of ceramic ink zaffre, which is characterized in that it includes the following steps：
S1. raw material is weighed：Molar ratio by Co: Al: Si is (2 ~ 4):(2~2.5):(3 ~ 5) weigh cobalt source, silicon source and silicon respectively
Source；
S2. preliminary mixing：The raw material weighed is put into conical mixer and is tentatively mixed；
S3. powder is beaten：The raw material tentatively mixed is dropped in claw pulverizer and is further uniformly mixed, is made between each raw material fully
Contact；
S4. calcine：Beat powder after raw material calcined at 1130 DEG C ~ 1200 DEG C 2 ~ 3 it is small when；
S5. crush, refine：Semifinished product after calcining carries out extra-fine grinding processing, obtains the finished product of submicron order.
2. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that the cobalt source is oxidation
Cobalt, cobalt carbonate or cobalt hydroxide.
3. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that source of aluminium is hydroxide
Aluminium or calcined alumina.
4. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that the silicon source is quartz.
5. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that the cobalt source is through airflow milling
Machining is to fineness D100 no more than 10 μm.
6. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that source of aluminium is through airflow milling
Machining is to fineness D100 no more than 5 μm.
7. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that the silicon source is through airflow milling
Machining is to fineness D100 no more than 10 μm.
8. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that in step S1, the original
Material further includes magnesia and/or zinc oxide.
9. the preparation method of ceramic ink zaffre as described in claim 1, which is characterized in that in step S1, the original
Material does not include mineralizer.
10. a kind of ceramic ink zaffre is prepared by any one of the claim 1-9 preparation methods.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256901A (en) * | 2019-06-12 | 2019-09-20 | 魏炎梅 | A kind of preparation method of cobalt blue ceramic glaze special-purpose ink |
| CN110804393A (en) * | 2019-12-12 | 2020-02-18 | 西北永新涂料有限公司 | Preparation method of high-temperature-resistant coating with self-cleaning performance |
| CN111057401A (en) * | 2019-12-12 | 2020-04-24 | 西北永新涂料有限公司 | Method for preparing cobalt blue/layered silicate clay mineral hybrid pigment by solid-phase method |
| CN111171601A (en) * | 2020-02-24 | 2020-05-19 | 中国科学院兰州化学物理研究所 | Method for preparing cobalt blue hybrid pigment by using quartz removed in natural mineral purification process |
| CN111218131A (en) * | 2019-12-12 | 2020-06-02 | 西北永新涂料有限公司 | Preparation method for preparing cobalt blue/clay mineral hybrid pigment by solid-phase method |
| CN111621169A (en) * | 2020-06-05 | 2020-09-04 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
| CN112876881A (en) * | 2021-02-03 | 2021-06-01 | 中山市华山高新陶瓷材料有限公司 | Cobalt blue pigment based on five-membered system and solid-phase preparation method thereof |
| CN114656802A (en) * | 2022-03-17 | 2022-06-24 | 湖州学院 | Blue ceramic pigment and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256901A (en) * | 2019-06-12 | 2019-09-20 | 魏炎梅 | A kind of preparation method of cobalt blue ceramic glaze special-purpose ink |
| CN110804393A (en) * | 2019-12-12 | 2020-02-18 | 西北永新涂料有限公司 | Preparation method of high-temperature-resistant coating with self-cleaning performance |
| CN111057401A (en) * | 2019-12-12 | 2020-04-24 | 西北永新涂料有限公司 | Method for preparing cobalt blue/layered silicate clay mineral hybrid pigment by solid-phase method |
| CN111218131A (en) * | 2019-12-12 | 2020-06-02 | 西北永新涂料有限公司 | Preparation method for preparing cobalt blue/clay mineral hybrid pigment by solid-phase method |
| CN110804393B (en) * | 2019-12-12 | 2021-06-29 | 西北永新涂料有限公司 | Preparation method of high-temperature-resistant coating with self-cleaning performance |
| CN111218131B (en) * | 2019-12-12 | 2021-08-03 | 西北永新涂料有限公司 | Preparation method for preparing cobalt blue/clay mineral hybrid pigment by solid-phase method |
| CN111057401B (en) * | 2019-12-12 | 2021-09-28 | 西北永新涂料有限公司 | Method for preparing cobalt blue/layered silicate clay mineral hybrid pigment by solid-phase method |
| CN111171601A (en) * | 2020-02-24 | 2020-05-19 | 中国科学院兰州化学物理研究所 | Method for preparing cobalt blue hybrid pigment by using quartz removed in natural mineral purification process |
| CN111621169A (en) * | 2020-06-05 | 2020-09-04 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
| CN111621169B (en) * | 2020-06-05 | 2021-06-08 | 江苏拜富科技股份有限公司 | Method for blending high-stability pigment for heat-resistant porcelain pot |
| CN112876881A (en) * | 2021-02-03 | 2021-06-01 | 中山市华山高新陶瓷材料有限公司 | Cobalt blue pigment based on five-membered system and solid-phase preparation method thereof |
| CN114656802A (en) * | 2022-03-17 | 2022-06-24 | 湖州学院 | Blue ceramic pigment and preparation method thereof |
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Application publication date: 20180529 |
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| RJ01 | Rejection of invention patent application after publication |