CN100577745C - High color density fine inorganic pigment, method for producing the same and inorganic pigment ink composition thereof - Google Patents
High color density fine inorganic pigment, method for producing the same and inorganic pigment ink composition thereof Download PDFInfo
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- CN100577745C CN100577745C CN 200610106160 CN200610106160A CN100577745C CN 100577745 C CN100577745 C CN 100577745C CN 200610106160 CN200610106160 CN 200610106160 CN 200610106160 A CN200610106160 A CN 200610106160A CN 100577745 C CN100577745 C CN 100577745C
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Abstract
The invention provides high color concentration micronized inorganic paint and the preparation method. The method is that the water glass is adopted to cover the praseodymium salt or praseodymium oxide and the mineralizer to form the grain, and is mixed with the monox (SiO2) and the zirconia to burn into praseodymium yellow inorganic paint to improve the color concentration of the paint after micronization of the inorganic paint. The invention also provides an inorganic paint ink composite for spray ink printing, which comprises the high color concentration micronized inorganic paint, the dispersant, humectant and other additives.
Description
[technical field under the invention]
The present invention relates to a kind of mineral dye (pigment) and manufacture method thereof, be particularly to a kind of manufacture method of high color density fine inorganic pigment, and the ink jet ink composition that contains this kind mineral dye.
[prior art]
Jet printing technique system directly the use ink gun with the ink spray printing on base material (for example pottery, glass etc.) develop the color through high temperature sintering again, utilize the digitizing technology mode fast the picture proof design directly to be exported and shorten the process time, to save traditional web plate and make time-histories and expense, also save a large amount of half tones storage area simultaneously.
With regard to mineral dye, possess high color density and high dispersive stability after need possessing miniaturization with regard to a good ceramic spray printing, therefore when pigment in the miniaturization process, depth of shade can not be disperseed and colour killing because grinding, and depth of shade still must be kept behind the sintering; In addition, the fine inorganic pigment ink set also must be preserved for a long time, can not block spray orifice because environmental change produces particle aggregation.
The general ink for ink-jet print required rerum natura demand of filling a prescription comprises characteristics such as viscosity, solubleness, component compatibility and base material be moistening.In addition, ink must possess rapid drying, high color density and characteristic such as wear-resisting on base material, must not block via a China ink spray orifice and ink-jet smoothly simultaneously.Though ink-jet technology day by day ripe and be widely used in industrial, yet need high temperature sintering commodity etc. after still not having " mineral dye decentralized " ink for ink-jet print actuals product so far and being applied to pottery, glass and other spray printing.
Mention in patent and the document that spray printing develops the color through high temperature sintering in ceramic surface again as US Patent No.5273575 utilization " lysotype inorganic salts " ink for ink-jet print though have.Though and US Patent No.5443628 and US Patent No.5407474 mention " mineral dye decentralized " ink for ink-jet print, its particle diameter must be between 20～200nm to avoid blocking problems such as spray orifice, settlement on storage and redispersion, but, make that " mineral dye decentralized " ink for ink-jet print always can't commercialization because mineral dye can produce the problem of pigment because of the miniaturization colour killing in the miniaturization process.
Tradition praseodymium yellow pigment synthesis mode is with zirconium white (ZrO
2), silicon oxide (SiO
2), praseodymium oxalate (Pr
2(C
2O
4)
3) and mineralizer burn till praseodymium yellow via 800～1100 ℃ of high temperature.Burning till reaction mechanism is SiO
2Generate volatile halogenated with the mineralizer effect earlier, diffuse to ZrO then
2With Pr
2(C
2O
4)
3Reaction generates praseodymium yellow, so SiO
2With Pr
2(C
2O
4)
3Mix evenly more, the praseodymium yellow effect that obtains is good more.Mention general wire mark technology its best coloring intensity particle diameter D of praseodymium yellow pigment in InterceramVol.53 (2004) document
50Be 5.9 microns, D
90It is 12.2 microns, because of containing unreacted silicon oxide and zirconium white and white intermediate silicon oxide zirconium (ZrSiO in the pigment particles center
2), cause praseodymium yellow pigment in grinding the miniaturization process, because of the exposed dilution of white color produces the colour killing situation.In conventional pigment technology, above-mentioned four kinds of raw material uniform mixing are burnt till praseodymium yellow pigment, the pigment particle size that obtains is about 2～6 microns, after miniaturization the pigment colour killing serious, therefore must its manufacture method of improvement.
In another traditional technology, earlier with mineralizer and Pr
2(C
2O
4)
3Behind the uniform mixing, again with ZrO
2And SiO
2Puddle roughly, be fired into the higher praseodymium yellow pigment of colourity, but this practice can't be efficient with Pr
2(C
2O
4)
3Close with mineralizer.
Therefore, industry is needed a kind of method for making of high color density fine inorganic pigment badly, it can improve praseodymium yellow pigment reactivity, and still can have high color density after the pigment miniaturization, and this high color density fine inorganic pigment can be applicable to the spray ink Printing inorganic pigment ink.
[summary of the invention]
The object of the present invention is to provide a kind of high color density fine inorganic pigment with and manufacture method.
The present invention utilizes water glass with praseodymium salt or Praseodymium trioxide (Pr
6O
11) coat a plurality of particulates of formation with mineralizer, wherein mineralizer comprises Sodium Fluoride, ammonium chloride, sodium-chlor, lithium fluoride, Repone K, barium fluoride or its combination; Again should a plurality of particulates and silicon oxide (SiO
2) and zirconium white (ZrO
2) mix and burn till, obtain high color density praseodymium yellow pigment; After this pigment ground with shredder at a slow speed, obtain micron grain size pigment, after making pigment reach stabilization with wet type miniaturization grinding and the grinding of adjustment dispersion agent prescription again, obtain time micrometer/nanometer particle diameter pigment concentrated solution, still can keep high color density after the pigment miniaturization of the present invention.
Another object of the present invention is to provide a kind of spray ink Printing inorganic pigment ink composition, comprise above-mentioned high color density fine inorganic pigment, dispersion agent, wetting Agent for Printing Inks and other additive.
In above-mentioned mineral dye technology, being added with of water glass helps improve praseodymium yellow pigment reactivity, because the water glass unit price is cheap and can directly burn till removal fully under the situation at high temperature, can not cause the burden of ink set, therefore mineral dye of the present invention has the praseodymium yellow depth of shade of raising and can be applicable to ceramic spray printing inorganic pigment ink.
[embodiment]
Make Praseodymium trioxide (Pr among the present invention
6O
11) approaching with the mineralizer distance, as mineralizer activation SiO
2Back and ZrO
2Produce ZrSiO
2During crystalline phase, contiguous Pr
6O
11Pr
4+Can replace Zr fast
4+Position on lattice generates the praseodymium yellow lattice.Work as Pr
6O
11With Zr
4+When distance is far away, Pr
4+Be difficult for replacing Zr
4+To make the praseodymium yellow pigment content reduce unreacted white initiator SiO
2With ZrO
2And white intermediate ZrSiO
2Occupy the majority, white can expose and dilute pigment when miniaturization, forms the colour killing phenomenon.
Therefore, the present invention utilizes water glass with praseodymium salt or Praseodymium trioxide (Pr
6O
11) coat a plurality of particulates of formation with mineralizer, make Pr
6O
11Close with mineralizer, again with a plurality of particulates and silicon oxide (SiO
2) and zirconium white (ZrO
2) mix and burn till, can improve praseodymium yellow pigment reactivity, reduce unreacted white initiator SiO
2With ZrO
2And white intermediate ZrSiO
2Ratio, obtain high color density praseodymium yellow pigment.
Mineral dye manufacture method of the present invention is earlier with 1～15 weight parts water glass, 2～15 weight part Praseodymium trioxide (Pr
6O
11) and 2～10 weight part mineralizer mixed grindings 5～15 minutes, pulverize with 95～110 ℃ of heat baking backs again, make water glass coating Praseodymium trioxide and mineralizer form a plurality of particulates, wherein mineralizer comprises Sodium Fluoride, ammonium chloride, sodium-chlor, lithium fluoride, Repone K, barium fluoride or its combination.
Then, again with above-mentioned a plurality of particulates and 15～40 weight part SiO
2And 40～70 weight part ZrO
2Mix forming mixture, this mixture is burnt till, firing temperature is 850～1100 ℃, and firing time is 0.5～7 hour, obtains pigment after burning till.Earlier with shredder ground pigment at a slow speed, form micron grain size pigment, its particle diameter is 1～6 μ m.And then utilize wet grinding and formula adjustment to grind formation time micrometer/nanometer particle diameter pigment, its particle diameter is less than 300nm, wherein wet grinding and formula adjustment grind and use dispersion agent and grinding medium, and dispersion agent for example is that (manufacturers: BYK), grinding medium for example is a yttrium zirconium pearl to BYK154.
Have high depth of shade via the resulting miniaturization praseodymium yellow of aforesaid method pigment, can measure by colourimeter, its depth of shade is 0.53～0.59.
The present invention utilizes water glass and guarantees pr except can be used as carrier
4+Enough in ZrSiO
2Lattice replaces Zr smoothly
4+Position on lattice obtains high reactivity praseodymium yellow lattice, and can still keep the high color density characteristic after the pigment miniaturization.In addition, remove, so the present invention not only can improve the praseodymium yellow depth of shade and also not pollute simultaneously because water glass can utilize high temperature to burn till fully.
High color density fine inorganic pigment of the present invention can be used for the spray printing composition for ink, its composition comprises by resulting high color density fine inorganic pigment 1～40 weight part of above-mentioned method for making, dispersion agent 1～20 weight part, wetting Agent for Printing Inks 0.5～20 weight part and other additive 0～10 weight part, wherein dispersion agent for example is BYK154 (BYK of manufacturers), wetting Agent for Printing Inks for example is DEG (Dietyleneglycol, Tedia company), 1,5PDO (1,5Patanediol, Lancaster Synthesis), this other additive is interfacial agent or other additive, be preferably the additive of adjusting capillary interfacial agent and being applicable to spray printing, for example BYK180, BYK333, BYK192 (BYK of manufacturers) and SFL465 (the Air Product of manufacturers) etc.Above-mentioned composition for ink can be used for high temperature resistant 650～1350 ℃ or fast light base material, for example ceramic tile, pottery, glass, mural painting base material or outdoor spray printing base material etc., and behind high temperature sintering, still can keep high color density on the base material.
High color density fine inorganic pigment manufacture method provided by the present invention, can overcome the problem that previous praseodymium yellow pigment synthesis mode can't overcome, because the painted application of traditional praseodymium yellow pigment most application pottery, utilize artificial or wire mark technology with pigment application in pottery surface sintering quality, its best color development pigment particle size is about about 2～6 microns.And ceramic decoration technology of new generation is ceramic digital spraying print technology, directly utilize ink gun with the mineral dye spray printing on pottery, because the about 30 microns sizes of ink gun spray orifice and its density height of mineral dye, therefore mineral dye must miniaturization to time micron big or small (＜300nm), just can make the pigment stable dispersion in the ink set and be applied to jet printing technique.Tradition praseodymium yellow pigment is because its best color development particle diameter is 2～6 microns; therefore miniaturization to time micron size can produce the colour killing phenomenon; the present invention can solve micronize praseodymium yellow pigment colour killing problem, produces high color density fine praseodymium yellow pigment, and can be applicable to spray printing, wire mark and coating process.
[embodiment 1]
With 5 weight part Pr
6O
11, 2 weight part ammonium chlorides, 1 weight part barium fluoride, 3 weight part Repone K, add 2.75 weight parts water glass behind the thorough mixing, ground simultaneously 5～15 minutes, again with 95～110 ℃ of heat bakings and pulverize.Add 22 weight part silicon oxide and 49 weight part zirconium whites, burnt till 6 hours at 980 ℃ behind the thorough mixing.Burn till the back and use shredder grinding toner to 1～6 micron grain sizes at a slow speed earlier, utilize wet grinding and formula adjustment to be ground to again less than 300nm, obtain the mineral dye concentrated solution, wherein (manufacturers: BYK), the dispersion agent dosage is 0.5 for the ratio to pigment to dispersion agent use BYK154, and grinding medium uses yttrium zirconium pearl, grinding its concentrated solution mineral dye of back is 20 weight percents (wt%), median size is 148nm, and viscosity is 2.9cps, and surface tension is 44.2mN/m.
[embodiment 1a]
Utilize spray gun to be sprayed on the base material, the spray gun label is ANEST IWATA W-61, and model is SPRAY GUN.
Ink set preparation: get that 20wt% concentrated solution 89.1 grams add water to 100 grams among the embodiment 1, pigment content is 17.82wt%, the gained slurry irritated behind spray gun, evenly be sprayed on the 5cm * 5cm ceramic tile test piece that has been coated with glaze, finish after 40～50 minutes with 1100～1150 ℃ of high temperature sinterings, measure the depth of shade of ceramic tile again with colourimeter, measuring result sees also table 1.
[embodiment 1b]
Utilize the ink-jet printer spray printing to base material, use ink gun to be hp 626 models (hot gas alveolitoid ink gun).
Ink set preparation: get 20wt% concentrated solution 89.1 weight parts among the embodiment 1, add wetting Agent for Printing Inks DEG (Dietyleneglycol, Tedia company) 1 weight part, and (manufacturers: BYK) (manufacturers: BYK) 0.6 weight part, the ink viscosity that obtains are 3.2cps for 0.3 weight part, BYK192 to add additive B YK333; With ink hp 626 jet-printing heads of packing into, and load onto spray printing board spray printing, control ink-jet number, make pigment be coated with even spray printing on the 5cm of glaze * 5cm ceramic tile, finish after 40～50 minutes with 1100～1150 ℃ of high temperature sinterings, measure the depth of shade of ceramic tile again with colourimeter, measuring result sees also table 1.
[embodiment 1c]
Utilize the ink-jet printer spray printing to base material, use ink gun to be Xaar 128 models (piezo-electric type ink gun).
Ink set preparation and spray printing, sintering process are measured the depth of shade of ceramic tile with embodiment 1b with colourimeter after finishing, measuring result sees also table 1.
[comparative example 1]
With 5 weight part Pr
6O
11, 2 weight part ammonium chlorides, 1 weight part barium fluoride, 3 weight part Repone K, 22 weight part silicon oxide and 49 weight part zirconium whites, burnt till 6 hours at 980 ℃ behind the thorough mixing.To burn till the back toner and earlier be ground to 1～6 micron grain size with shredder at a slow speed, and utilize wet grinding and formula adjustment to be ground to less than 200nm again, and obtain the mineral dye concentrated liquid prescription, wherein dispersion agent uses BYK154, grinding medium use yttrium zirconium pearl.Grind the result and show that its median size is 148nm, viscosity is 2.8cps, and surface tension is 44.2mN/m.
[comparative example 1a]
Concentrated solution in the comparative example 1 is allocated formula of size according to the mode identical with embodiment 1a, and with utilize spray gun to spray the sintering colour developing according to the mode identical with embodiment 1a, measure the depth of shade of ceramic tile after finishing with colourimeter, measuring result sees also table 1.
[comparative example 1b]
Utilize the ink-jet printer spray printing to base material, use ink gun to be hp 626 models.
Ink set preparation: get 20wt% concentrated solution 89.1 weight parts in the comparative example 1, add wetting Agent for Printing Inks DEG (Dietyleneglycol, Tedia company) 1 weight part, and (manufacturers: BYK) (manufacturers: BYK) 0.6 weight part, the ink viscosity that obtains are 3.2cps for 0.3 weight part, BYK192 to add additive B YK333; With ink hp 626 jet-printing heads of packing into, and load onto spray printing board spray printing, control ink-jet number, make pigment be coated with even spray printing on the 5cm of glaze * 5cm ceramic tile, finish after 40～50 minutes with 1100～1150 ℃ of high temperature sinterings, measure the depth of shade of ceramic tile again with colourimeter, measuring result sees also table 1.
[comparative example 1c]
Utilize the ink-jet printer spray printing to base material, use ink gun to be Xaar 128 models.
Ink set preparation and spray printing, sintering process are measured the depth of shade of ceramic tile with comparative example 1b with colourimeter after finishing, measuring result sees also table 1.
The depth of shade measuring method is that spray printing same amount yellow ultramarine is on ceramic tile, again with ceramic tile via High Temperature Furnaces Heating Apparatus sintering quality, measure the yellow color lump concentration in sintering front and back with ColorTron, and Lab value, L represents the brightness (lightness of a color) of color, a and b then represent the form and aspect (hue) and the chroma (chroma) of color, the scope of a from represent green-a to expression red+a, the scope of b is then from representing that blueness-b is to expression xanchromatic+b, the yellow of the big more expression praseodymium yellow of b value pigment is yellow more, and use chromascope ColorTron to measure depth of shade, the big more color representation of depth of shade value is better.
Depth of shade measuring result such as the following table 1 of the foregoing description 1a, 1b, 1c and comparative example 1a, 1b, 1c are listed:
Table 1 yellow ultramarine particle diameter and colour developing situation
Can learn by table 1, the b value of embodiment 1a, 1b and 1c is all than the comparative example height, the mineral dye manufacture method that expression the present invention adds water glass, the fine inorganic pigment praseodymium yellow depth of shade that it obtains is 0.53～0.55, does not add traditional mineral dye manufacture method praseodymium yellow depth of shade height of water glass.
Though the present invention has disclosed preferred embodiment as above; right its is not in order to qualification the present invention, any those who are familiar with this art, without departing from the spirit and scope of the invention; when can doing a little change and retouching, so the present invention's protection domain attached claim after looking defines and is as the criterion.
Claims (17)
1. the manufacture method of a mineral dye comprises:
Provide water glass to coat praseodymium salt or Praseodymium trioxide and mineralizer and form a plurality of particulates, wherein this mineralizer comprises Sodium Fluoride, ammonium chloride, sodium-chlor, lithium fluoride, Repone K, barium fluoride or its combination;
Should mix the formation mixture with silicon oxide and zirconium white by a plurality of particulates;
This mixture is burnt till formation pigment; And
With extremely inferior micron of this pigment grind or nanometer particle size pigment.
2. the manufacture method of mineral dye according to claim 1, wherein the weight part of this praseodymium salt or Praseodymium trioxide is 2～15, and the weight part of this mineralizer is 2～10, and the weight part of this water glass is 1～15.
3. the manufacture method of mineral dye according to claim 1, wherein this silicon oxide weight part is 15～40, this zirconium white weight part is 40～70.
4. the manufacture method of mineral dye according to claim 1 also is included in and forms before this nanometer particle size pigment, forms micron grain size pigment.
5. as the manufacture method of mineral dye as described in the claim 4, wherein this micron grain size is 1～6 μ m.
6. the manufacture method of mineral dye according to claim 1, wherein this nanometer particle size is less than 300nm.
7. the manufacture method of mineral dye according to claim 1, wherein this water glass is removed when this mixture burns till.
8. the manufacture method of mineral dye according to claim 1 also comprises this praseodymium salt or Praseodymium trioxide and this mineralizer and this water glass mixed grinding 5～15 minutes, pulverizes with 95～110 ℃ of heat baking backs and obtains this a plurality of particulates.
9. as the manufacture method of mineral dye as described in the claim 4, also comprise grinding this micron grain size pigment is made time micron or nanometer particle size pigment concentrated solution with wet grinding and formula adjustment.
10. as the manufacture method of mineral dye as described in the claim 9, wherein this wet grinding and formula adjustment grind and use dispersion agent and grinding medium.
11. the high color density fine inorganic pigment that the manufacture method of the described mineral dye of claim 1 is made, its depth of shade are 0.53～0.59, particle diameter is less than 300nm.
12. as high color density fine inorganic pigment as described in the claim 11, it is used for spray ink Printing, screen painting or coating process.
13. the inorganic pigment ink composition that spray ink Printing is used comprises:
As high color density fine inorganic pigment as described in the claim 11;
Dispersion agent;
Wetting Agent for Printing Inks; And
Other additives.
14. as spray ink Printing inorganic pigment ink composition as described in the claim 13, wherein this additive is an interfacial agent.
15. as spray ink Printing inorganic pigment ink composition as described in the claim 13, wherein this additive is for adjusting capillary interfacial agent and being applicable to the additive of spray printing.
16. as spray ink Printing inorganic pigment ink composition as described in the claim 13, it is used for high temperature resistant or fast light base material.
17. as spray ink Printing inorganic pigment ink composition as described in the claim 16, wherein this high temperature resistant base material is ceramic tile, pottery, glass, mural painting base material or other outdoor spray printing base materials, and can high temperature resistantly be 650～1350 ℃.
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|---|---|---|---|
| CN 200610106160 CN100577745C (en) | 2006-07-20 | 2006-07-20 | High color density fine inorganic pigment, method for producing the same and inorganic pigment ink composition thereof |
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|---|---|---|---|
| CN 200610106160 CN100577745C (en) | 2006-07-20 | 2006-07-20 | High color density fine inorganic pigment, method for producing the same and inorganic pigment ink composition thereof |
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| CN100577745C true CN100577745C (en) | 2010-01-06 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093084B (en) * | 2010-12-24 | 2013-04-24 | 广东东鹏陶瓷股份有限公司 | Zirconium silicate coated ceramic pigment for inkjet printing and preparation method thereof |
| CN102584340B (en) * | 2012-03-19 | 2013-05-08 | 中山市华山高新陶瓷材料有限公司 | Agate red ceramic pigment for ink-jet printing and preparation method thereof |
| CN102675967B (en) * | 2012-05-08 | 2014-01-15 | 中山大学 | Water-based ceramic three-dimensional pattern printing ink and preparation method thereof |
| ITVR20120207A1 (en) * | 2012-10-18 | 2014-04-19 | Projecta Engineering S R L | DECORATION LINE FOR CERAMIC PRODUCTS |
| TWI461491B (en) * | 2012-12-28 | 2014-11-21 | Ind Tech Res Inst | Dispersion, inkjet ink, and manufacturing the inkjet ink |
| CN103145453A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Praseodymium yellow material for ceramic ink and preparation method thereof |
| CN103272677B (en) * | 2013-05-22 | 2015-01-14 | 袁伟 | Method for preparing nano particles and application thereof |
| CN103342917B (en) * | 2013-07-04 | 2015-07-15 | 西安电子科技大学 | Yellow ceramic ink for ink-jet printing |
| CN105835554A (en) * | 2016-03-29 | 2016-08-10 | 王兆进 | Method for preparing attapulgite digital printing wallpaper |
| CN109161227A (en) * | 2018-08-23 | 2019-01-08 | 佛山市三水区康立泰无机合成材料有限公司 | A kind of preparation method of the reddish brown colorant of ceramic ink jet |
| CN108862292A (en) * | 2018-09-10 | 2018-11-23 | 江西师范大学 | A method of regulation silicon dioxide microsphere partial size |
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| US3756840A (en) * | 1970-04-22 | 1973-09-04 | Thann & Mulhouse | Zirconium pigments |
| RO66383A2 (en) * | 1975-02-28 | 1978-12-15 | Inst De Chimie | PROCESS FOR THE PREPARATION OF YELLOW CERAMIC PIGMENTS BASED ON ZIRCONIUM SILICATE |
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