CN107936697A - A kind of high dispersive, fine grain whiteware ink raw powder's production technology - Google Patents
A kind of high dispersive, fine grain whiteware ink raw powder's production technology Download PDFInfo
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- CN107936697A CN107936697A CN201711338244.0A CN201711338244A CN107936697A CN 107936697 A CN107936697 A CN 107936697A CN 201711338244 A CN201711338244 A CN 201711338244A CN 107936697 A CN107936697 A CN 107936697A
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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 high dispersive, fine grain whiteware ink raw powder's production technology, including：Prepare the ZrOCl2 aqueous solutions of 0.05-0.3mol/l；Prepare 2 aqueous solutions of Mg (NO3) of 0.05-0.3mol/l；By the isometric addition of Mg (NO3) 2 aqueous solutions into ZrOCl2 aqueous solutions；The aqueous solutions mixed with ZrOCl2 of Mg (NO3) 2 are stirred by mixer, mixing speed 200-300r/min, 5-8min is stirred, to stirring evenly；Tissuemat E is added into uniform mixed liquor, Tissuemat E is the 1-1.5% of 2 mass of Mg (NO3)；Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10-11 to control pH value, and aqueous solution is heated, and controls 80-90 DEG C of water temperature, keeps 3-4h, there is Precipitation；Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2-3 times；Precipitation after washing is positioned in 80-90 DEG C of baking oven and is dried；Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2 ceramic ink powders.The color of ceramic ink is enriched, also enriches the preparation method for preparing whiteware ink, technique is simple.
Description
Technical field
The present invention relates to ceramic technology field, more particularly to a kind of high dispersive, the system of fine grain whiteware ink powder
Preparation Method.
Background technology
Inkjet printing technology is a kind of ceramic decoration technology of great application value, still, realizes inkjet printing technology
One of key is the preparation of ceramic ink.
Existing ceramic ink, when forming ceramic ink system, often appears as shakiness since the particle diameter of powder is larger
Fixed, easy conglomeration, causes quality greatly to receive influence.And existing ceramic ink higher price, color is abundant not enough, especially
It is whiteware ink whiteness and covering power it is inadequate.
The content of the invention
In view of this, the present invention provides a kind of high dispersive, fine grain whiteware ink raw powder's production technology, enrich
The color of ceramic ink, while the preparation method for preparing whiteware ink is also enriched, technique is simple, the powder prepared
Body particle diameter is small, when being dispersed in ink system, has polymolecularity.
A kind of high dispersive, fine grain whiteware ink raw powder's production technology, the described method includes：
Prepare the ZrOCl2 aqueous solutions of 0.05-0.3mol/l；
Prepare 2 aqueous solutions of Mg (NO3) of 0.05-0.3mol/l；
By the isometric addition of Mg (NO3) 2 aqueous solutions into ZrOCl2 aqueous solutions；
The aqueous solutions mixed with ZrOCl2 of Mg (NO3) 2 are stirred by mixer, mixing speed 200-300r/min,
5-8min is stirred, to stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is the 1-1.5% of 2 mass of Mg (NO3)；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10-11 to control pH value, and aqueous solution is heated,
80-90 DEG C of water temperature is controlled, 3-4h is kept, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2-3 times；
Precipitation after washing is positioned in 80-90 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2 ceramic ink powders.
Preferably, the method is：
Prepare the ZrOCl2 aqueous solutions of 0.1-0.2mol/l；
Prepare 2 aqueous solutions of Mg (NO3) of 0.1-0.2mol/l；
By the isometric addition of Mg (NO3) 2 aqueous solutions into ZrOCl2 aqueous solutions；
The aqueous solutions mixed with ZrOCl2 of Mg (NO3) 2 are stirred by mixer, mixing speed 220-280r/min,
6-7min is stirred, to stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is the 1.2-1.4% of 2 mass of Mg (NO3)；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10 to control pH value, and aqueous solution is heated, and is controlled
84-88 DEG C of water temperature, keeps 3h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2 times；
Precipitation after washing is positioned in 82-86 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2 ceramic ink powders.
Preferably, the method is：
Prepare the ZrOCl2 aqueous solutions of 0.15mol/l；
Prepare 2 aqueous solutions of Mg (NO3) of 0.15mol/l；
By the isometric addition of Mg (NO3) 2 aqueous solutions into ZrOCl2 aqueous solutions；
The aqueous solutions mixed with ZrOCl2 of Mg (NO3) 2 are stirred by mixer, mixing speed 260r/min, stirred
7min, to stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is the 1.3% of 2 mass of Mg (NO3)；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 11 to control pH value, and aqueous solution is heated, and is controlled
87 DEG C of water temperature, keeps 4h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 3 times；
Precipitation after washing is positioned in 85 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2 ceramic ink powders.
Preferably, the Tissuemat E molecular weight is 1500-1800.
Preferably, the Tissuemat E molecular weight is 1700.
Preferably, the heat treatment is that sediment is carried out 750-800 DEG C of temperature lower calcination, calcines 1-1.5h.
Preferably, the heat treatment is that sediment is carried out 780 DEG C of temperature lower calcinations, calcines 1.2h.
Preferably, it is described to be ground to machine by grinding, then sieve, powder is ground again in sieve.
Preferably, the MgO-ZrO2 ceramic inks diameter of particle is 7-9nm.
It is provided by the invention the present invention provides a kind of high dispersive, fine grain whiteware ink raw powder's production technology,
Enrich the color of ceramic ink, while also enrich the preparation method for preparing whiteware ink, technique is simple, cost compared with
Low, the diameter of particle prepared is small, when being dispersed in ink system, has polymolecularity.
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.
Zr element because of metal its with mechanical benefits such as good mechanics and biological property, in new material development field
With very important status, particularly in terms of ceramic ink, it is as whiteware powder.But existing zr element
Ceramic ink is when powder makes, its particle diameter or of a relatively high, may thus cause ceramic ink system to produce unstable
Property.This method passes through modified technique so that the ceramic ink powder come into output has fine grain, has height in ink system
It is scattered.In the following, it is illustrated in connection with specific embodiments.
Embodiment 1
Prepare the ZrOCl of 0.3mol/l2Aqueous solution；
Prepare the Mg (NO of 0.3mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 300r/min, stirring
5min, to stirring evenly；
The Tissuemat E that molecular weight is 1500 is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2Quality
1%；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10 to control pH value, and aqueous solution is heated, and is controlled
80 DEG C of water temperature, keeps 4h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 3 times；
Precipitation after washing is positioned in 90 DEG C of baking oven and is dried；
Dried sediment is subjected to 750 DEG C of temperature lower calcinations into sediment is about to, 1.5h is calcined, then passes through grinding
Machining, then sieves, powder is ground again in sieve, obtains MgO-ZrO2Ceramic ink powder.
Embodiment 2
Prepare the ZrOCl of 0.05mol/l2Aqueous solution；
Prepare the Mg (NO of 0.05mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 200r/min, stirring
8min, to stirring evenly；
The Tissuemat E that molecular weight is 1800 is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2Quality
1.5%；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 11 to control pH value, and aqueous solution is heated, and is controlled
90 DEG C of water temperature, keeps 3h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2 times；
Precipitation after washing is positioned in 80 DEG C of baking oven and is dried；
Dried sediment is subjected to 800 DEG C of temperature lower calcinations, calcines 1h, is then machined by grinding, then mistake
Sieve, powder is ground again in sieve, obtains MgO-ZrO2Ceramic ink powder.
Embodiment 3
Prepare the ZrOCl of 0.1mol/l2Aqueous solution；
Prepare the Mg (NO of 0.1mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 220r/min, stirring
7min, to stirring evenly；
The Tissuemat E that molecular weight is 1700 is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2Quality
1.4%；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10 to control pH value, and aqueous solution is heated, and is controlled
88 DEG C of water temperature, keeps 3h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2 times；
Precipitation after washing is positioned in 86 DEG C of baking oven and is dried；
Dried sediment is subjected to 780 DEG C of temperature lower calcinations, calcines 1.2h, then machined by grinding, then
Sieve, powder is ground again in sieve, obtains MgO-ZrO2Ceramic ink powder.
Embodiment 4
Prepare the ZrOCl of 0.2mol/l2Aqueous solution；
Prepare the Mg (NO of 0.2mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 280r/min, stirring
6min, to stirring evenly；
The Tissuemat E that molecular weight is 1600 is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2Quality
1.2%；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10 to control pH value, and aqueous solution is heated, and is controlled
84 DEG C of water temperature, keeps 3h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2 times；
Precipitation after washing is positioned in 82 DEG C of baking oven and is dried；
Dried sediment is subjected to 760 DEG C of temperature lower calcinations, calcines 1.4h, then machined by grinding, then
Sieve, powder is ground again in sieve, obtains MgO-ZrO2Ceramic ink powder.
Embodiment 5
Prepare the ZrOCl of 0.15mol/l2Aqueous solution；
Prepare the Mg (NO of 0.15mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 260r/min, stirring
7min, to stirring evenly；
The Tissuemat E that molecular weight is 1800 is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2Quality
1.3%；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 11 to control pH value, and aqueous solution is heated, and is controlled
87 DEG C of water temperature, keeps 4h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 3 times；
Precipitation after washing is positioned in 85 DEG C of baking oven and is dried；
Dried sediment is subjected to 740 DEG C of temperature lower calcinations, calcines 1.6h, then machined by grinding, then
Sieve, powder is ground again in sieve, obtains MgO-ZrO2Ceramic ink powder.
The ceramic ink powder that embodiment 1 to 6 is produced, is added in ink system, to its particle diameter and stability into
Row test, test result such as following table：
| D (particle diameter)/nm | Place 12h (sediment) | Place 24h (sediment) | |
| Embodiment 1 | 8.94 | Nothing | Nothing |
| Embodiment 2 | 9.02 | Nothing | Nothing |
| Embodiment 3 | 7.45 | Nothing | Nothing |
| Embodiment 4 | 6.83 | Nothing | Nothing |
| Embodiment 5 | 8.21 | Nothing | Nothing |
As can be seen that split particle diameter is in 7-9nm in table, and by not settling for a long time, prepared high dispersive,
Fine grain whiteware ink powder, technique is simple, and cost is relatively low.
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 (9)
1. a kind of high dispersive, fine grain whiteware ink raw powder's production technology, it is characterised in that the described method includes：
Prepare the ZrOCl of 0.05-0.3mol/l2Aqueous solution；
Prepare the Mg (NO of 0.05-0.3mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 200-300r/min, stirs 5-
8min, to stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2The 1-1.5% of quality；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10-11 to control pH value, and aqueous solution is heated, control
80-90 DEG C of water temperature, keeps 3-4h, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2-3 times；
Precipitation after washing is positioned in 80-90 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2Ceramic ink powder.
2. preparation method as claimed in claim 1, it is characterised in that the method is：
Prepare the ZrOCl of 0.1-0.2mol/l2Aqueous solution；
Prepare the Mg (NO of 0.1-0.2mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 220-280r/min, stirs 6-
7min, to stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2The 1.2-1.4% of quality；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 10 to control pH value, and aqueous solution is heated, and controls water temperature
84-88 DEG C, 3h is kept, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 2 times；
Precipitation after washing is positioned in 82-86 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2Ceramic ink powder.
3. preparation method as claimed in claim 1, it is characterised in that the method is：
Prepare the ZrOCl of 0.15mol/l2Aqueous solution；
Prepare the Mg (NO of 0.15mol/l3)2Aqueous solution；
By Mg (NO3)2The isometric addition of aqueous solution is to ZrOCl2In aqueous solution；
By Mg (NO3)2With ZrOCl2The aqueous solution of mixing is stirred by mixer, mixing speed 260r/min, stirs 7min,
To stirring evenly；
Tissuemat E is added into uniform mixed liquor, Tissuemat E is Mg (NO3)2The 1.3% of quality；
Again toward ammonium hydroxide is added in the solution for be mixed with Tissuemat E, it is 11 to control pH value, and aqueous solution is heated, and controls water temperature
87 DEG C, 4h is kept, there is Precipitation；
Aqueous solution with precipitation is poured out, is filtered by vacuum, precipitation surface is cleaned with acetone, cleans 3 times；
Precipitation after washing is positioned in 85 DEG C of baking oven and is dried；
Dried sediment is heat-treated, is then ground, obtains MgO-ZrO2Ceramic ink powder.
4. the preparation method as described in claim 1-3 is any, it is characterised in that：The Tissuemat E molecular weight is 1500-
1800。
5. preparation method as claimed in claim 4, it is characterised in that：The Tissuemat E molecular weight is 1700.
6. the preparation method as described in claim 1-3 is any, it is characterised in that：The heat treatment is that sediment is carried out 750-
800 DEG C of temperature lower calcinations, calcine 1-1.5h.
7. preparation method as claimed in claim 6, it is characterised in that：The heat treatment is that sediment is carried out 780 DEG C of temperature
Lower calcining, calcines 1.2h.
8. the preparation method as described in claim 1-3 is any, it is characterised in that：It is described to be ground to machine by grinding, so
After sieve, powder is ground again in sieve.
9. the preparation method as described in claim 1-3 is any, it is characterised in that：The MgO-ZrO2Ceramic ink diameter of particle
For 7-9nm.
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| CN201711338244.0A CN107936697A (en) | 2017-12-14 | 2017-12-14 | A kind of high dispersive, fine grain whiteware ink raw powder's production technology |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033750A (en) * | 1987-12-26 | 1989-07-12 | 冶金部洛阳耐火材料研究所 | Pyroceramic oxide micropowder production method |
| CN1280882A (en) * | 2000-09-01 | 2001-01-24 | 清华大学 | Nm-class crystal oxide carried nickel catalyst and its preparing process |
| CN101481246A (en) * | 2009-02-24 | 2009-07-15 | 河北理工大学 | Preparation of ZrO2-Al2TiO5-MgO composite nano powder |
-
2017
- 2017-12-14 CN CN201711338244.0A patent/CN107936697A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033750A (en) * | 1987-12-26 | 1989-07-12 | 冶金部洛阳耐火材料研究所 | Pyroceramic oxide micropowder production method |
| CN1280882A (en) * | 2000-09-01 | 2001-01-24 | 清华大学 | Nm-class crystal oxide carried nickel catalyst and its preparing process |
| CN101481246A (en) * | 2009-02-24 | 2009-07-15 | 河北理工大学 | Preparation of ZrO2-Al2TiO5-MgO composite nano powder |
Non-Patent Citations (1)
| Title |
|---|
| 张小芳等: "沉淀剂对ZrO2(MgO)纳米粉体制备的影响", 《材料与冶金学报》 * |
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