CN103804993B - A kind of extra white aqueous ceramic jetted ink and preparation method thereof - Google Patents

A kind of extra white aqueous ceramic jetted ink and preparation method thereof Download PDF

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CN103804993B
CN103804993B CN201310610589.2A CN201310610589A CN103804993B CN 103804993 B CN103804993 B CN 103804993B CN 201310610589 A CN201310610589 A CN 201310610589A CN 103804993 B CN103804993 B CN 103804993B
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ink
sol
ceramic
colloidal sol
extra white
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CN103804993A (en
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毛海燕
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FOSHAN CAIGUI NEW MATERIAL CO., LTD.
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FOSHAN MINGZHAO TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

A kind of extra white aqueous ceramic jetted ink, its beramic color is the colloidal sol that the presoma of zirconic presoma and silicon oxide is prepared by sol-gel method.The present invention adopts sol-gel method to prepare the beramic color of white, particle diameter is thinner, and there is good sphericity, not only solve the grinding technique problem of the long-time and highly energy-consuming of traditional ceramics jetted ink, and better remain active group by sol gel reaction, beramic color of the present invention can be sintered at lesser temps, and overcoming zirconium white pigment in prior art needs 1500 DEG C of high temperature sinterings could sinter the technical barrier of fastening attachment.The preparation method of a kind of extra white aqueous ceramic jetted ink of the present invention comprises and prepares colloidal sol step and grinding steps, its preparation method is simple, and obtained extra white aqueous ceramic jetted ink has that whiteness is high, ink-jet is effective, be applicable to the advantages such as high precision ink jet printing head.

Description

A kind of extra white aqueous ceramic jetted ink and preparation method thereof
Technical field
The present invention relates to ceramic ink jet technical field, particularly relate to a kind of extra white aqueous ceramic jetted ink and preparation method thereof.
Background technology
Ceramic ink jet technology ink-jet printed technology is applied to the technology that ceramic surface carries out decorating, it is that ceramic powder to be formed is made ceramic ink, utilize printer that the ceramic ink configured directly is printed to the shaping surface of architectural pottery, then at sintering, wherein, the shape of molding and geometrical dimension are by computer control.The ceramic ink that current most domestic Ceramics Enterprises uses is mainly based on the ceramic ink that Spain Esmalglass ~ itaca, Ferro Deng Jijia offshore company of the U.S. produce, and domestic ceramic ink is the main ceramic ink jet ink released for 2010 with Science and Technology Development Co., Ltd. of the Ming Dynasty then.Ceramic ink jet ink both domestic and external is mainly based on blue, brown, yellow, tangerine look, golden yellow, black, pink, and the ordering of its passage in ceramic ink jet printer is also different according to the product of different manufacturers and have different orderings.On the whole, the color of above several ceramic ink jet ink can meet the Production requirement of most of producer and most product substantially, can produce Protean ceramic ink jet product.But, in recent years due to the popular of ceramic ink jet product and the impact of market homogeneity, some producers producing high-end personalized ceramic product are badly in need of on the chromatic series of ceramic ink jet ink, increase extra white color, enrich product, simultaneously the personalization features of outstanding product.
And due to ceramic ink jet ink be the ceramic ink that ceramic powder to be formed makes solution shape, utilize printer that the ceramic ink configured directly is printed to the shaping surface of architectural pottery, and then sinter, owing to being different from ceramic coating in the special preparation of ceramic ink jet ink and use-pattern, both belong to two kinds of different technical fields, the technology in ceramic coating is made to be difficult to directly apply to ceramic ink jet ink, therefore, for existing problems of the prior art, need badly and provide a kind of extra white ceramic ink jet ink technology to seem particularly important.
Summary of the invention
The object of the invention is to avoid weak point of the prior art and provide that a kind of whiteness is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method's simple extra white aqueous ceramic jetted ink.
Object of the present invention is achieved through the following technical solutions:
There is provided a kind of extra white aqueous ceramic jetted ink, its beramic color is the colloidal sol that the presoma of zirconic presoma and silicon oxide is prepared by sol-gel method,
Wherein, in described colloidal sol, silicon oxide and zirconic mole ratio are for being less than or equal to 1:1, or the content of silicon oxide is 0.
Preferably, in described colloidal sol, the mole ratio of zirconium white and silicon oxide is 4:1, and extra white aqueous ceramic jetted ink sintering temperature is now lower, and whiteness is high, and ink-jet sintering effect is good.
Preferably, described zirconic presoma is zirconium oxychloride or oxygen zirconic acid amine; The presoma of described silicon oxide is the one of tetraethoxy-silicane, tetramethoxy-silicane and water glass or two or more, and wherein, the modulus of water glass is equal to, or greater than 2.
Above-mentioned extra white aqueous ceramic jetted ink, containing deionized water, aqueous dispersant, tensio-active agent, water-miscible organic solvent and ink addition agent.
Preferably, a kind of extra white aqueous ceramic jetted ink is grouped into by the one-tenth of following weight percent:
Deionized water 20 ~ 55%
Colloidal sol 35 ~ 60%
Aqueous dispersant and tensio-active agent 2 ~ 10%
Water-miscible organic solvent 2-10%
Ink addition agent 2 ~ 6%
Wherein, the weight of colloidal sol calculates with the dry weight after its calcination.
Preferred, a kind of extra white aqueous ceramic jetted ink is grouped into by the one-tenth of following weight percent:
Deionized water 23%
Colloidal sol 60%
Aqueous dispersant and tensio-active agent 10%.
Water-miscible organic solvent 2%
Ink addition agent 5% .
Another is preferred, and a kind of extra white aqueous ceramic jetted ink is grouped into by the one-tenth of following weight percent:
Deionized water 25 ~ 50%
Colloidal sol 40 ~ 60%
Aqueous dispersant and tensio-active agent 4 ~ 10%
Water-miscible organic solvent 2 ~ 10%
Ink addition agent 3 ~ 6%
Wherein, the weight of colloidal sol calculates with the dry weight after its calcination.
Preferred, a kind of extra white aqueous ceramic jetted ink is grouped into by the one-tenth of following weight percent:
Deionized water 35%
Colloidal sol 45%
Aqueous dispersant and tensio-active agent 8%.
Water-miscible organic solvent 8%
Ink addition agent 4%.
Wherein, described water-miscible organic solvent is ethylene glycol, ethylene glycol monomethyl ether; diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, propylene glycol monomethyl ether; dipropylene glycol monomethyl ether; thanomin, diethanolamine, trolamine; methyl-sulphoxide; morpholine, nitro morpholine, the one of nitrosomorpholine and N-formyl morpholine or two or more.
Another object of the present invention is to avoid weak point of the prior art and provide a kind of and prepare that above-mentioned whiteness is high, ink-jet is effective, be applicable to high precision ink jet printing head, the preparation method of preparation method's simple extra white aqueous ceramic jetted ink.
Another object of the present invention is achieved through the following technical solutions:
A kind of preparation method of extra white aqueous ceramic jetted ink is provided, includes following steps:
Step a. colloidal sol
The presoma of zirconic presoma and silicon oxide synchronously joins in the ethanolic soln of 50% lentamente, stir while add, after adding completely, stir hydrolysis reaction 24 hours, leave standstill 6 little layereds afterwards, after abandoning supernatant liquid, add deionized water in stirring, then leave standstill 6 little layereds, abandon supernatant liquid, repeat above process, until washing pH value is neutral, obtain colloidal sol;
The density of sol system is adjusted to 1.28 ~ 1.5g/cm by the mode of releasing supernatant liquid by the colloidal sol after above-mentioned washing by step a1. 3, add aqueous dispersant, tensio-active agent reduce the viscosity of system and carry out modification to sol surface simultaneously, while adding surface-modifying agent, use high speed dispersor to stir, after reinforced, continue high-speed stirring 45 ~ 65 minutes; This step effectively can reduce the viscosity of system, improves the stably dispersing performance of system simultaneously;
After the sol surface modification completely that step a2. is modified, more slowly add aqueous organic solvent, slowly add ink addition agent afterwards, continue high-speed stirring 55 ~ 65 minutes;
Step b. just grinds
The mixture obtained by step a2 first carries out grinding distribution through ball mill, grind after 1.5 ~ 10 hours and obtain just grinding material, milling time and the sol gel reaction time proportional, be ground to sol particle granularity and reach 0.1 ~ 1 micron, obtain ceramic ink jet ink, keep in Dark Place for subsequent use.
In step b, described ball mill employing diameter is that the zirconium oxide bead of 0.3mm grinds.
Preferably, in step b, described ball mill employing diameter is that the zirconium oxide bead of 0.3mm grinds.
Beneficial effect of the present invention:
A kind of extra white aqueous ceramic jetted ink, its beramic color is the colloidal sol that the presoma of zirconic presoma and silicon oxide is prepared by sol-gel method, wherein, in described colloidal sol, silicon oxide and zirconic mole ratio are for being less than or equal to 1:1, or the content of silicon oxide is 0.The present invention adopts sol-gel method to prepare the beramic color of white, particle diameter is thinner, and there is good sphericity, can be good at by sol-gel method the initial size controlling material simultaneously, preparation method is simple, not only solve the grinding technique problem of the long-time and highly energy-consuming of traditional ceramics jetted ink, be applicable to high precision ink jet printing head, ensure high resolving power and the high precision of ceramic ink jet, and better remain active group by sol gel reaction, beramic color of the present invention can be sintered at lesser temps, overcoming zirconium white pigment in prior art needs 1500 DEG C of high temperature sinterings could sinter the technical barrier of fastening attachment.Meanwhile, the mole number of the silicon oxide in the present invention is not higher than zirconic mole number, since it effectively reduces ink cost, reduces sintering temperature, can ensure required whiteness again.When the mole number of silicon oxide is 0, beramic color is zirconia sol, and now, the whiteness of extra white aqueous ceramic jetted ink of the present invention is the highest.
The preparation method of a kind of extra white aqueous ceramic jetted ink of the present invention comprises and prepares colloidal sol step and grinding steps, its preparation method is simple, and obtained extra white aqueous ceramic jetted ink has that whiteness is high, ink-jet is effective, be applicable to the advantages such as high precision ink jet printing head.
Embodiment
The invention will be further described with the following Examples.
embodiment 1
The present embodiment a kind of extra white aqueous ceramic jetted ink is provided, its beramic color is the colloidal sol that the presoma of zirconic presoma and silicon oxide is prepared by sol-gel method, wherein, the mole number of 0:1≤silicon oxide in described colloidal sol: zirconic mole number≤1:1, in the present embodiment, colloidal sol contains silica sol, and silicon oxide in colloidal sol and zirconic mole ratio are less than or equal to 1:1, and other compositions are substantially identical with common water borne ceramic ink jet ink.
In the present embodiment, above-mentioned zirconic presoma is zirconium oxychloride or oxygen zirconic acid amine, and certain zirconic presoma also can be other materials, as long as it can use sol-gel method to prepare zirconia sol; The presoma of above-mentioned silicon oxide is the one of tetraethoxy-silicane, tetramethoxy-silicane and water glass or two or more, wherein, the modulus of water glass is equal to, or greater than 2, the presoma of certain silicon oxide also can be other materials, as long as it can use sol-gel method to prepare silica sol.
The colloidal sol that beramic color of the present invention is chosen to be zirconium white and silicon oxide is applied to ceramic ink jet ink relative to prior art and non-obvious, although existing in prior art, zirconium white is used in ceramic coating, but ceramic coating and ceramic ink jet ink are two different technical fields, the use of ceramic coating is the ceramic film of heat setting one-tenth after being directly overlying on metal base, its objective is the not viscosity in order to improve metal base, wear resistance and thermal oxidation resistance aging, zirconium white wherein has also been the hardness and the wear resistance that improve ceramic coating, ceramic ink jet ink is then utilize printer spray printing on pottery, pottery after spray printing sinters again, the technical problem that the zirconium white of extra white aqueous ceramic jetted ink of the present invention solves prepares the beramic color of extra white, and energy and water, water-miscible organic solvents etc. are miscible use well.And the zirconium white of colloidal sol of the present invention and the ratio of silicon oxide, be also the research and development of contriver's creativeness, not simple limited number of time experiment is available.
embodiment 2
A kind of extra white aqueous ceramic jetted ink of the present embodiment, except other compositions of beramic color are deionized water, aqueous dispersant, tensio-active agent, water-miscible organic solvent and ink addition agent, this extra white aqueous ceramic jetted ink is grouped into by the one-tenth of following weight percent:
Deionized water 20 ~ 55%
Colloidal sol 35 ~ 60%
Aqueous dispersant and tensio-active agent 2 ~ 10%
Water-miscible organic solvent 2-10%
Ink addition agent 2 ~ 6%
Wherein, the weight of colloidal sol calculates with the dry weight of the zirconium white after ink calcination and silicon oxide, and the mole ratio of zirconium white and silicon oxide is 1:1.
Wherein, after the weight of deionized water, ink calcination, the dry weight of colloidal sol, aqueous dispersant and surface-active weight, the quality of water-miscible organic solvent and the weight sum of ink addition agent are gross weight, and the weight percent of each composition is multiplied by 100% calculating for its weight divided by gross weight.
The extra white aqueous ceramic jetted ink of the present embodiment, environmental protection and remain high resolving power and the high precision of ceramic ink jet technology well, both can use, also can use on U.S.'s α ursa minoris 512 type shower nozzle on Sai Er 1001 type shower nozzle.And the solid grain size that formed of the colloidal sol made evenly, more carefully, then in follow-up process of lapping, save milling time and raise the efficiency than traditional ceramics ink for ink-jet print, the more activity hydroxy sintering temperature in surface is lower simultaneously.
Described water-miscible organic solvent is ethylene glycol, ethylene glycol monomethyl ether, diethylene glycol monomethyl ether; triethylene glycol monomethyl ether; propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, thanomin; diethanolamine; trolamine, methyl-sulphoxide, morpholine; nitro morpholine, the one of nitrosomorpholine and N-formyl morpholine or two or more.
Described aqueous dispersant can be water-soluble polyacrylate, aqurous ployurethane acrylate etc., tensio-active agent mainly alkyl polyoxyethylene ether, polyoxyethylene nonylphenol ether etc., and polyethenoxy ether class nonionic surface active agent.
And ink addition agent mainly contains flow agent, or other can reduce capillary auxiliary agent, can be water miscible organosilicons etc.
The preparation method of above-mentioned a kind of extra white aqueous ceramic jetted ink, includes following steps:
Step a. colloidal sol
The presoma of zirconic presoma and silicon oxide synchronously joins in the ethanolic soln of 50% mass percent lentamente, stir while add, after material adds completely, stir hydrolysis reaction 24 hours, leave standstill 6 little layereds afterwards, after abandoning supernatant liquid, add deionized water and stir again, then leave standstill 6 little layereds, abandon supernatant liquid, repeat above process, until washing pH value is neutral, obtain colloidal sol;
Step a1.
The density of sol system is adjusted to 1.28 ~ 1.5g/cm by the mode of releasing supernatant liquid by the colloidal sol after above-mentioned washing 3, add aqueous dispersant, tensio-active agent reduce the viscosity of system and carry out modification to sol surface simultaneously, while adding surface-modifying agent, use high speed dispersor to stir, after reinforced, continue high-speed stirring 45 ~ 65 minutes; This step effectively can reduce the viscosity of system, improves the stably dispersing performance of system simultaneously;
Step a2.
After modified sol surface modification completely, more slowly add aqueous organic solvent, slowly add ink addition agent afterwards, continue high-speed stirring 55 ~ 65 minutes;
Step b. grinds
The mixture obtained by step a2 first carries out grinding distribution through ball mill, grind after 1.5 ~ 10 hours and obtain just grinding material, milling time and the sol gel reaction time proportional, be ground to the granularity of ceramic pigment in sol particle and reach 0.1 ~ 1 micron, obtain ceramic ink jet ink, keep in Dark Place for subsequent use.
The main technical schemes of the present embodiment is substantially the same manner as Example 1, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1, no longer repeats at this.
embodiment 3
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is also containing silane coupling agent, when preparing extra white aqueous ceramic jetted ink, coupling agent is added when adding water-miscible organic solvent, tensio-active agent, coupling agent mainly contains water miscible silane coupling agent, titanate coupling agent, specifically can be aminopropyl-triethoxy silicon, aminopropyl trimethoxy silicon, epoxypropyl triethoxysilicane, epoxypropyl trimethoxy silicon etc.
embodiment 4
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 25 ~ 50%
Colloidal sol 35 ~ 60%
Aqueous dispersant and tensio-active agent 4 ~ 10%
Water-miscible organic solvent 2 ~ 10%
Ink addition agent 3 ~ 6%
Wherein, be only made up of zirconia sol in described colloidal sol, the content of silicon oxide is 0.Do not add the presoma of silicon oxide when preparing colloidal sol, the extra white ceramic ink jet ink whiteness that the colloidal sol of this composition is obtained is very high.
embodiment 5
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 23%
Colloidal sol 60%
Aqueous dispersant and tensio-active agent 10%
Water-miscible organic solvent 2%
Ink addition agent 5%,
In the present embodiment, in described colloidal sol, the mole ratio of zirconium white and silicon oxide is 4:1, and extra white aqueous ceramic jetted ink sintering temperature is now lower, and whiteness is high, and ink-jet sintering effect is good.
The preparation method of extra white aqueous ceramic jetted ink in the present embodiment, zirconic presoma is zirconium oxychloride, and the presoma of silicon oxide is tetraethoxy-silicane.
embodiment 6
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 35%
Colloidal sol 45%
Aqueous dispersant and tensio-active agent 8%
Water-miscible organic solvent 8%
Ink addition agent 4%.
Extra white aqueous ceramic jetted ink of the present invention, more environmental protection, remain high resolving power and the high precision of ceramic ink jet technology well, both can use on Sai Er 1001 type shower nozzle, also can use on U.S.'s α ursa minoris 512 type shower nozzle.The preparation method of ceramic ink jet ink of the present invention, sol-gel method is adopted early stage to prepare whiteware pigment, particle diameter is thinner, there is good sphericity, can be good at by sol-gel method the initial size controlling material, solving traditional ceramics jetted ink needs long-time, the process of lapping of highly energy-consuming simultaneously, better remain active group by sol gel reaction simultaneously, can sinter at lesser temps.
embodiment 7
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 20%
Colloidal sol 39%
Aqueous dispersant and tensio-active agent 2%.
Water-miscible organic solvent 2%
Ink addition agent 2%.
The extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method is simple.
embodiment 8
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 14%
Colloidal sol 60%
Aqueous dispersant and tensio-active agent 10%
Water-miscible organic solvent 10%
Ink addition agent 6%.
The extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method is simple.
embodiment 9
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 50%
Colloidal sol 35%
Aqueous dispersant and tensio-active agent 6%
Water-miscible organic solvent 6%
Ink addition agent 3%.
The extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method is simple.
embodiment 10
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 46%
Colloidal sol 45%
Aqueous dispersant and tensio-active agent 4%
Water-miscible organic solvent 2%
Ink addition agent 5%.
The extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method is simple.
embodiment 11
The main technical schemes of the present embodiment is substantially identical with embodiment 1 or 2, the feature do not laid down a definition in the present embodiment, adopts the explanation in embodiment 1 or embodiment 2, no longer repeats at this.A kind of extra white aqueous ceramic jetted ink of the present embodiment is grouped into by the one-tenth of following weight percent:
Deionized water 25%
Colloidal sol 56%
Aqueous dispersant and tensio-active agent 8%
Water-miscible organic solvent 8%
Ink addition agent 3%.
The extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, be applicable to high precision ink jet printing head, preparation method is simple.
The experimental result of embodiment 5 to the embodiment 11 of extra white aqueous ceramic jetted ink of the present invention is as following table:
The test result that table 1 Sai Er GS12 shower nozzle 100% grayscale inkjet prints
As shown in Table 1, the extra white aqueous ceramic jetted ink whiteness of the present embodiment is high, ink-jet is effective, technique is simple, preparation energy consumption is low, cost-saving.
Finally should be noted that; above embodiment is only for illustration of technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.

Claims (10)

1. an extra white aqueous ceramic jetted ink, is characterized in that: its beramic color is the colloidal sol that the presoma of zirconic presoma and silicon oxide is prepared by sol-gel method,
Wherein, in described colloidal sol, silicon oxide and zirconic mole ratio are for being less than or equal to 1:1, or the content of silicon oxide is 0;
Described extra white ceramic water jetted ink is prepared by the following method:
Step a. colloidal sol
The presoma of zirconic presoma and silicon oxide synchronously joins in the ethanolic soln of 50% lentamente, stir while add, after adding, stir hydrolysis reaction 24 hours, leave standstill 6 little layereds afterwards, after abandoning supernatant liquid, add deionized water and leave standstill 6 little layereds in stirring again after 2 hours, abandon supernatant liquid, repeat above process, until washing pH value is neutral, obtain colloidal sol;
Step a1.
The density of sol system is adjusted to 1.28 ~ 1.5g/cm by the mode of releasing supernatant liquid by the colloidal sol after above-mentioned washing 3, add aqueous dispersant, tensio-active agent reduce the viscosity of system and carry out modification to sol surface simultaneously, while adding surface-modifying agent, use high speed dispersor to stir, after reinforced, continue high-speed stirring 45 ~ 65 minutes;
Step a2.
After modified sol surface modification completely, more slowly add aqueous organic solvent, slowly add ink addition agent afterwards, continue high-speed stirring 55 ~ 65 minutes;
Step b. just grinds
The mixture obtained by step a2 first carries out grinding distribution through ball mill, grind after 1.5 ~ 10 hours and obtain just grinding material, milling time and the sol gel reaction time proportional, be ground to the granularity of ceramic pigment in sol particle and reach 0.1 ~ 1 micron, obtain ceramic ink jet ink, keep in Dark Place for subsequent use.
2. a kind of extra white aqueous ceramic jetted ink according to claim 1, is characterized in that: in described colloidal sol, the mole ratio of zirconium white and silicon oxide is 4:1.
3. a kind of extra white aqueous ceramic jetted ink according to claim 1, is characterized in that: described zirconic presoma is zirconium oxychloride or fluorine zirconic acid amine;
The presoma of described silicon oxide is the one of tetraethoxy-silicane, tetramethoxy-silicane and water glass or two or more, and wherein, the modulus of water glass is equal to, or greater than 2.
4. a kind of extra white aqueous ceramic jetted ink according to claim 1, is characterized in that: containing deionized water, aqueous dispersant, tensio-active agent, water-miscible organic solvent and ink addition agent.
5. a kind of extra white aqueous ceramic jetted ink according to claim 4, is characterized in that: be grouped into by the one-tenth of following weight percent:
Deionized water 20 ~ 55%
Colloidal sol 35 ~ 60%
Aqueous dispersant and tensio-active agent 2 ~ 10%
Water-miscible organic solvent 2-10%
Ink addition agent 2 ~ 6%
Wherein, the weight of colloidal sol calculates with the dry weight after its calcination.
6. a kind of extra white aqueous ceramic jetted ink according to claim 5, is characterized in that: be grouped into by the one-tenth of following weight percent:
Deionized water 23%
Colloidal sol 60%
Aqueous dispersant and tensio-active agent 10%
Water-miscible organic solvent 2%
Ink addition agent 5% .
7. a kind of extra white aqueous ceramic jetted ink according to claim 4, is characterized in that: be grouped into by the one-tenth of following weight percent:
Deionized water 25 ~ 50%
Colloidal sol 40 ~ 60%
Aqueous dispersant and tensio-active agent 4 ~ 10%
Water-miscible organic solvent 2 ~ 10%
Ink addition agent 3 ~ 6%
Wherein, the weight of colloidal sol calculates with the dry weight after its calcination.
8. a kind of extra white aqueous ceramic jetted ink according to claim 7, is characterized in that: be grouped into by the one-tenth of following weight percent:
Deionized water 35%
Colloidal sol 45%
Aqueous dispersant and tensio-active agent 8%
Water-miscible organic solvent 8%
Ink addition agent 4%.
9. a kind of extra white aqueous ceramic jetted ink according to claim 4 ~ 8 any one, is characterized in that: described water-miscible organic solvent is ethylene glycol, ethylene glycol monomethyl ether; diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, propylene glycol monomethyl ether; dipropylene glycol monomethyl ether; thanomin, diethanolamine, trolamine; methyl-sulphoxide; morpholine, nitro morpholine, the one of nitrosomorpholine and N-formyl morpholine or two or more.
10. a preparation method for extra white aqueous ceramic jetted ink, is characterized in that: extra white aqueous ceramic jetted ink as described in claim 1 to 9 any one, and its preparation method includes following steps:
Step a. colloidal sol
The presoma of zirconic presoma and silicon oxide synchronously joins in the ethanolic soln of 50% lentamente, stir while add, after adding, stir hydrolysis reaction 24 hours, leave standstill 6 little layereds afterwards, after abandoning supernatant liquid, add deionized water and leave standstill 6 little layereds in stirring again after 2 hours, abandon supernatant liquid, repeat above process, until washing pH value is neutral, obtain colloidal sol;
Step a1.
The density of sol system is adjusted to 1.28 ~ 1.5g/cm by the mode of releasing supernatant liquid by the colloidal sol after above-mentioned washing 3, add aqueous dispersant, tensio-active agent reduce the viscosity of system and carry out modification to sol surface simultaneously, while adding surface-modifying agent, use high speed dispersor to stir, after reinforced, continue high-speed stirring 45 ~ 65 minutes;
Step a2.
After modified sol surface modification completely, more slowly add aqueous organic solvent, slowly add ink addition agent afterwards, continue high-speed stirring 55 ~ 65 minutes;
Step b. just grinds
The mixture obtained by step a2 first carries out grinding distribution through ball mill, grind after 1.5 ~ 10 hours and obtain just grinding material, milling time and the sol gel reaction time proportional, be ground to the granularity of ceramic pigment in sol particle and reach 0.1 ~ 1 micron, obtain ceramic ink jet ink, keep in Dark Place for subsequent use.
CN201310610589.2A 2013-11-27 2013-11-27 A kind of extra white aqueous ceramic jetted ink and preparation method thereof Active CN103804993B (en)

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CN105131713A (en) * 2015-09-17 2015-12-09 上海大学 Yellow nano ceramic printing ink
CN106189514B (en) * 2016-08-04 2019-10-11 佛山科学技术学院 Black blue and white coloring material aqueous dispersing agent and preparation method and application for inkjet printing
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CN107151483B (en) * 2017-05-31 2020-08-18 华南理工大学 Ink for ink-jet printing, preparation method thereof and zirconia film printed by same
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CN107474631A (en) * 2017-09-19 2017-12-15 常州市卜诺赛机电技术有限公司 A kind of ink-jet ceramic ink and preparation method thereof
CN107778991B (en) * 2017-11-02 2021-05-04 武汉理工大学 Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof
CN111454615A (en) * 2020-06-09 2020-07-28 佛山市扬子颜料有限公司 Glaze ink for ink-jet printing and preparation method thereof

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