CN107955458A - A kind of blue powder preparation method for ceramic ink - Google Patents
A kind of blue powder preparation method for ceramic ink Download PDFInfo
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- CN107955458A CN107955458A CN201711353092.1A CN201711353092A CN107955458A CN 107955458 A CN107955458 A CN 107955458A CN 201711353092 A CN201711353092 A CN 201711353092A CN 107955458 A CN107955458 A CN 107955458A
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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
- C09D11/322—Pigment inks
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Abstract
The invention discloses a kind of blue powder preparation method for ceramic ink, including：The AlCl3 aqueous solutions of 0.1-0.5mol/l are prepared, it is spare；2 aqueous solutions of Co (NO3) of 0.05-0.2mol/l are prepared, it is spare；The NH3-H2O aqueous solutions of 2-4mol/l are prepared, it is spare；AlCl3 aqueous solutions are added in Co (NO3) 2 aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is stirred, obtains solution a；NH3-H2O aqueous solutions are added into solution a, obtain b solution, the pH value for controlling b solution is 11.5-12.5, and stirs to without precipitation and produce；B solution is placed in reaction kettle and is heated, holding pressure is 0.5-0.6MPa, and reaction time 16-20h, then depressurizes, be cooled to room temperature, there is Precipitation；B solution with precipitation is centrifuged, centrifugal speed 12000-15000r/min, obtains sediment；Sediment is placed in drier and is dried, drying temperature is 20-40 DEG C, drying time 16-24h；Dried sediment is ground, obtains CoAl2O4 powders.Solves CoAl very well2O4The purity of powder is not high, and particle diameter is big, and preparation process is complicated, and condition is harsh, it is of high cost the problems such as.
Description
Technical field
The present invention relates to ceramic ink technical field, more particularly to a kind of blue powder preparation side for ceramic ink
Method.
Background technology
With the fast development of industry, the type of merchandize of in the market is also more and more, and many commodity are also increasingly pursued high
Quality.
Ceramic ink is always institute of offshore company ridge as the key component as ceramic ink jet printing technology, its core
It is disconnected so that domestic ceramic ink holds at high price.And wherein, the core of ceramic ink is ceramic powder again, so ceramic powder
Body technique is only the key of ceramic ink jet printing technology.
CoAl2O4The one kind of powder as blue powder, it is using relatively broad, still, existing CoAl2O4Powder is pure
Degree is not high, and the particle diameter made is larger, is applying in ceramic ink, is embodied in colourity heterogeneity, poor dispersion.It is and existing
Some preparation method complex process, condition is harsh, causes its production cost higher, marketing degree is low.
The content of the invention
In view of this, the present invention provides a kind of blue powder preparation method for ceramic ink, it is solved well
CoAl2O4The purity of powder is not high, and particle diameter is big, and preparation process is complicated, and condition is harsh, it is of high cost the problems such as.
A kind of blue powder preparation method for ceramic ink, the described method includes：
The AlCl3 aqueous solutions of 0.1-0.5mol/l are prepared, it is spare；
2 aqueous solutions of Co (NO3) of 0.05-0.2mol/l are prepared, it is spare；
The NH3-H2O aqueous solutions of 2-4mol/l are prepared, it is spare；
AlCl3 aqueous solutions are added in Co (NO3) 2 aqueous solution so that Co2+ is 1 with Al3+ molar ratios:2, to solution into
Row stirring, obtains solution a；
NH3-H2O aqueous solutions are added into solution a, obtain b solution, the pH value for controlling b solution is 11.5-12.5, and is stirred
Mix to without precipitation and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.5-0.6MPa, reaction time 16-20h, so
After depressurize, be cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 12000-15000r/min, obtains sediment；
Sediment is placed in drier and is dried, drying temperature is 20-40 DEG C, drying time 16-24h；
Dried sediment is ground, obtains CoAl2O4 powders.
Preferably, the method is：
The AlCl3 aqueous solutions of 0.2-0.4mol/l are prepared, it is spare；
2 aqueous solutions of Co (NO3) of 0.08-0.15mol/l are prepared, it is spare；
The NH3-H2O aqueous solutions of 3-4mol/l are prepared, it is spare；
AlCl3 aqueous solutions are added in Co (NO3) 2 aqueous solution so that Co2+ is 1 with Al3+ molar ratios:2, to solution into
Row stirring, obtains solution a；
NH3-H2O aqueous solutions are added into solution a, obtain b solution, the pH value for controlling b solution is 11.8-12.2, and is stirred
Mix to without precipitation and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.52-0.58MPa, reaction time 17-19h,
Then depressurize, be cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 13000-14000r/min, obtains sediment；
Sediment is placed in drier and is dried, drying temperature is 24-36 DEG C, drying time 18-22h；
Dried sediment is ground, obtains CoAl2O4 powders.
Preferably, the method is：
The AlCl3 aqueous solutions of 0.3mol/l are prepared, it is spare；
2 aqueous solutions of Co (NO3) of 0.12mol/l are prepared, it is spare；
The NH3-H2O aqueous solutions of 4mol/l are prepared, it is spare；
AlCl3 aqueous solutions are added in Co (NO3) 2 aqueous solution so that Co2+ is 1 with Al3+ molar ratios:2, to solution into
Row stirring, obtains solution a；
NH3-H2O aqueous solutions are added into solution a, obtain b solution, the pH value for controlling b solution is 12, and is stirred to without heavy
Form sediment and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.55MPa, and reaction time 18h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 13500r/min, obtains sediment；
Sediment is placed in drier and is dried, drying temperature is 28 DEG C, drying time 20h；
Dried sediment is ground, obtains CoAl2O4 powders.
Preferably, further include and sediment progress alcohol is washed, alcohol washes number as 3-4 times, then dries.
Preferably, the alcohol that the alcohol is washed is ethanol, its concentration is 2-5mol/l.
Preferably, the CoAl2O4 powder purities are 92-99%.
Preferably, the CoAl2O4 powder purities are 99%.
Preferably, the CoAl2O4 powder granules are 5-8um.
It is provided by the invention that the present invention provides a kind of blue powder preparation method for ceramic ink, this method technique
Simply, condition is more gentle, low manufacture cost, and the CoAl prepared2O4The purity of powder is high, and particle diameter is small, can be in ceramics
High degree of dispersion in ink, and colourity is good.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is part of the embodiment of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's all other embodiments obtained without making creative work, belongs to
The scope of protection of the invention.
It should be appreciated that ought use in this specification and in the appended claims, term " comprising " and "comprising" instruction
Described feature, entirety, step, operation, the presence of element and/or component, but it is not precluded from one or more of the other feature, whole
Body, step, operation, element, component and/or its presence or addition for gathering.
It will be further appreciated that the term "and/or" used in description of the invention and the appended claims is
Refer to any combinations and all possible combinations of one or more of the associated item listed, and including these combinations.
Embodiment 1
Prepare the AlCl of 0.1mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.2mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 4mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 12.5, and is stirred to nothing
Precipitation produces；
B solution is placed in reaction kettle and is heated, holding pressure is 0.6MPa, and reaction time 16h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 12000r/min, obtains sediment；
Sediment is placed in drier and is dried, drying temperature is 40 DEG C, drying time 16h；
Dried sediment is ground, obtains CoAl2O4Powder.
Embodiment 2
Prepare the AlCl of 0.5mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.05mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 2mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 11.5, and is stirred to nothing
Precipitation produces；
B solution is placed in reaction kettle and is heated, holding pressure is 0.5MPa, and reaction time 20h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 15000r/min, obtains sediment；
Sediment is placed in drier and is dried, drying temperature is 20 DEG C, drying time 24h；
Dried sediment is ground, obtains CoAl2O4Powder.
Embodiment 3
Prepare the AlCl of 0.2mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.15mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 3mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 11.8, and is stirred to nothing
Precipitation produces；
B solution is placed in reaction kettle and is heated, holding pressure is 0.58MPa, and reaction time 19h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 14000r/min, obtains sediment, then use 5mol/
The ethanol of l carries out alcohol and washes, and alcohol washes number as 3 times；
Sediment is placed in drier and is dried, drying temperature is 36 DEG C, drying time 18h；
Dried sediment is ground, obtains CoAl2O4Powder.
Embodiment 4
Prepare the AlCl of 0.4mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.08mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 4mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 12.2, and is stirred to nothing
Precipitation produces；
B solution is placed in reaction kettle and is heated, holding pressure is 0.52MPa, and reaction time 17h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 13000r/min, obtains sediment, then use 2mol/
The ethanol of l carries out alcohol and washes, and alcohol washes number as 4 times；
Sediment is placed in drier and is dried, drying temperature is 24 DEG C, drying time 22h；
Dried sediment is ground, obtains CoAl2O4Powder.
Embodiment 5
Prepare the AlCl of 0.3mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.12mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 4mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 12, and stir to without heavy
Form sediment and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.55MPa, and reaction time 18h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 13500r/min, obtains sediment, then use 4mol/
The ethanol of l carries out alcohol and washes, and alcohol washes number as 5 times；
Sediment is placed in drier and is dried, drying temperature is 28 DEG C, drying time 20h；
Dried sediment is ground, obtains CoAl2O4Powder.
Comparative example 1
Prepare the AlCl of 0.6mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.06mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 1mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 13, and stir to without heavy
Form sediment and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.7MPa, and reaction time 22h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 110000r/min, obtains sediment, Ran Houyong
The ethanol of 1mol/l carries out alcohol and washes, and alcohol washes number as 5 times；
Sediment is placed in drier and is dried, drying temperature is 50 DEG C, drying time 15h；
Dried sediment is ground, obtains CoAl2O4Powder.
Comparative example 2
Prepare the AlCl of 0.05mol/l3Aqueous solution, it is spare；
Prepare the Co (NO of 0.3mol/l3)2Aqueous solution, it is spare；
Prepare the NH of 5mol/l3‐H2O aqueous solutions, it is spare；
By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is carried out
Stirring, obtains solution a；
NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 11, and stir to without heavy
Form sediment and produce；
B solution is placed in reaction kettle and is heated, holding pressure is 0.4MPa, and reaction time 14h, is then depressurized,
It is cooled to room temperature, there is Precipitation；
B solution with precipitation is centrifuged, centrifugal speed 160000r/min, obtains sediment, Ran Houyong
The ethanol of 6mol/l carries out alcohol and washes, and alcohol washes number as 2 times；
Sediment is placed in drier and is dried, drying temperature is 10 DEG C, drying time 28h；
Dried sediment is ground, obtains CoAl2O4Powder.
The CoAl that embodiment 1 to 6 is produced with comparative example 1 to 22O4Powder carries out purity and particle diameter test characterization,
Test result such as following table：
| D (particle diameter)/um (average) | CoAl2O4 powders (%) | |
| Embodiment 1 | 6.87 | 93% |
| Embodiment 2 | 8.03 | 92% |
| Embodiment 3 | 6.19 | 97% |
| Embodiment 4 | 6.83 | 95% |
| Embodiment 5 | 5.12 | 99% |
| Comparative example 1 | 9.34 | 87% |
| Comparative example 2 | 8.98 | 83% |
The CoAl prepared according to can be seen that this method in table2O4Powder purity is 92-99%, and highest can reach
99%, CoAl2O4Powder granule is 5-8um, than the CoAl of contrast test2O4Powder whether purity or on particle diameter all
There is larger lifting, this method technique is simple, and condition is more gentle, low manufacture cost, and the CoAl prepared2O4Powder
Purity is high, and particle diameter is small, can in ceramic ink high degree of dispersion, and colourity is good.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
It is described in detail herein, applies specific case and the principle of the present invention and embodiment are explained
State, above example is only intended to help the method and its core concept for understanding the present invention；Meanwhile for the general skill of this area
Art personnel, according to the thought of the present invention, there will be changes in specific embodiments and applications, in conclusion this
Description should not be construed as limiting the invention.
It is apparent to those skilled in the art that for convenience and simplicity of description, the system of foregoing description
With the specific work process of unit, the corresponding process in preceding method embodiment is may be referred to, details are not described herein.
Claims (8)
- A kind of 1. blue powder preparation method for ceramic ink, it is characterised in that the described method includes：Prepare the AlCl of 0.1-0.5mol/l3Aqueous solution, it is spare；Prepare the Co (NO of 0.05-0.2mol/l3)2Aqueous solution, it is spare；Prepare the NH of 2-4mol/l3‐H2O aqueous solutions, it is spare；By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is stirred, Obtain solution a；NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 11.5-12.5, and stir to nothing Precipitation produces；B solution is placed in reaction kettle and is heated, holding pressure is 0.5-0.6MPa, and reaction time 16-20h, then subtracts Pressure, is cooled to room temperature, there is Precipitation；B solution with precipitation is centrifuged, centrifugal speed 12000-15000r/min, obtains sediment；Sediment is placed in drier and is dried, drying temperature is 20-40 DEG C, drying time 16-24h；Dried sediment is ground, obtains CoAl2O4Powder.
- 2. preparation method as claimed in claim 1, it is characterised in that the method is：Prepare the AlCl of 0.2-0.4mol/l3Aqueous solution, it is spare；Prepare the Co (NO of 0.08-0.15mol/l3)2Aqueous solution, it is spare；Prepare the NH of 3-4mol/l3‐H2O aqueous solutions, it is spare；By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is stirred, Obtain solution a；NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 11.8-12.2, and stir to nothing Precipitation produces；B solution is placed in reaction kettle and is heated, holding pressure is 0.52-0.58MPa, reaction time 17-19h, then Decompression, is cooled to room temperature, there is Precipitation；B solution with precipitation is centrifuged, centrifugal speed 13000-14000r/min, obtains sediment；Sediment is placed in drier and is dried, drying temperature is 24-36 DEG C, drying time 18-22h；Dried sediment is ground, obtains CoAl2O4Powder.
- 3. preparation method as claimed in claim 1, it is characterised in that the method is：Prepare the AlCl of 0.3mol/l3Aqueous solution, it is spare；Prepare the Co (NO of 0.12mol/l3)2Aqueous solution, it is spare；Prepare the NH of 4mol/l3‐H2O aqueous solutions, it is spare；By AlCl3Aqueous solution adds Co (NO3)2In aqueous solution so that Co2+With Al3+Molar ratio is 1:2, solution is stirred, Obtain solution a；NH is added into solution a3‐H2O aqueous solutions, obtain b solution, and the pH value for controlling b solution is 12, and stirs to without precipitation and produce It is raw；B solution is placed in reaction kettle and is heated, holding pressure is 0.55MPa, and reaction time 18h, is then depressurized, cooling To room temperature, there is Precipitation；B solution with precipitation is centrifuged, centrifugal speed 13500r/min, obtains sediment；Sediment is placed in drier and is dried, drying temperature is 28 DEG C, drying time 20h；Dried sediment is ground, obtains CoAl2O4Powder.
- 4. the preparation method as described in claim 1-3 is any, it is characterised in that：Further include and sediment progress alcohol is washed, alcohol is washed secondary Number is 3-4 times, is then dried.
- 5. preparation method as claimed in claim 4, it is characterised in that：The alcohol that the alcohol is washed is ethanol, its concentration is 2-5mol/ l。
- 6. the preparation method as described in claim 1-3 is any, it is characterised in that：The CoAl2O4Powder purity is 92-99%.
- 7. preparation method as claimed in claim 6, it is characterised in that：The CoAl2O4Powder purity is 99%.
- 8. the preparation method as described in claim 1-3 is any, it is characterised in that：The CoAl2O4Powder granule is 5-8um.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210071225A (en) * | 2019-12-06 | 2021-06-16 | 한국세라믹기술원 | Manufacturing method of cobalt aluminum oxide |
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| CN102241528A (en) * | 2011-05-11 | 2011-11-16 | 景德镇陶瓷学院 | Process for preparing spherical nanometer spinel zaffre by hydrothermal method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102241528A (en) * | 2011-05-11 | 2011-11-16 | 景德镇陶瓷学院 | Process for preparing spherical nanometer spinel zaffre by hydrothermal method |
Non-Patent Citations (2)
| Title |
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| 卢希龙等: "尖晶石型纳米CoAl2O4色料水热合成工艺研究", 《人工晶体学报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210071225A (en) * | 2019-12-06 | 2021-06-16 | 한국세라믹기술원 | Manufacturing method of cobalt aluminum oxide |
| KR102352363B1 (en) * | 2019-12-06 | 2022-01-17 | 한국세라믹기술원 | Manufacturing method of cobalt aluminum oxide |
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Application publication date: 20180424 |