CN109749516A - A kind of inkjet printing photochromic ceramic ink and preparation method thereof - Google Patents
A kind of inkjet printing photochromic ceramic ink and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to architectural pottery technical fields, and in particular to a kind of inkjet printing photochromic ceramic ink and preparation method thereof.The described method includes: preparing photochromic colorant: Surfactant SDS is added into aluminium chloride and neodymium chloride mixed solution, later under water bath condition, oxalic acid solution is added dropwise while stirring, solution ph is adjusted again to 8~10, persistently stir 20~40min, the solution for there are a large amount of pale pink precipitatings is obtained, photochromic colorant will be obtained after solution ultrasound, washing, suction filtration, dry, calcining；It prepares photochromic ceramic ink: photochromic powder will be obtained after photochromic colorant ball milling, solvent, dispersing agent and water are added into gained powder, continue ball milling mixing and obtain suspension, suspension ultrasonic disperse is uniformly then obtained into photochromic ceramic ink.The photochromic ceramic ink stability of present invention preparation gained is good, different colors can be presented under different light sources, photochromic effect is good.
Description
Technical field
The invention belongs to architectural pottery technical fields, and in particular to a kind of photochromic ceramic ink of inkjet printing and its
Preparation method.
Background technique
Ceramic ink is that one kind is decorated by non-contact inkjet printing technique in architectural pottery surface, to meet ceramics
The new material of personalized customization demand has the characteristics that decorative effect is true to nature, grain pattern is rich and varied, is convenient for operation.It is photochromic
Ceramic ink refer to color can with the change of light source changed functionality ceramic ink.
The preparation of photochromic ceramic ink includes that colorant preparation and ink prepare two parts.About photochromic colorant
Preparation, " research of Er and the new ceramics camouflage paint of Nd combination coloring " (national engineering ceramics Annual Conference, 1999) text
It describes using silica, aluminium oxide, neodymia, erbium oxide as raw material, boric acid, sodium carbonate are mineralizer, using high temperature solid-state method
Neodymium type and erbium type discoloration colorant have been respectively synthesized at 1200 DEG C." study on the synthesis of neodymium ion doped calcium zirconate base discoloration colorant "
(South China Science & Engineering University, a 2014) text is reactant, ammonium carbonate as precipitating reagent using calcium nitrate, neodymium nitrate, zirconyl nitrate, is used
After coprecipitation synthesis presoma, the photochromic colorant that particle size is 1.425 μm is fired into through 1200 DEG C.About
The preparation of photochromic ink, Chinese invention patent " a kind of ink-jet photochromic low-temp ceramics ink and preparation method thereof "
(106336737 A of CN) disclose it is a kind of using silver nitrate, zinc nitrate, cerous nitrate as the photochromic compound of Material synthesis, it is auxiliary
Photochromic low-temp ceramics ink has been prepared with low temperature frit siccative, dispersing agent, surfactant etc..Chinese invention patent " one
Kind of rare earth function ceramics ink and preparation method thereof and production method " (104530831 A of CN) disclose it is a kind of with neodymia,
The photochromic ceramic ink of the compound oiliness of a variety of rare earth oxides such as erbium oxide.
Summary of the invention
The present invention in view of the deficiencies of the prior art, and it is an object of the present invention to provide a kind of photochromic ceramic ink of inkjet printing and
Preparation method.
For achieving the above object, the technical solution adopted by the present invention are as follows:
A kind of inkjet printing preparation method of photochromic ceramic ink, includes the following steps:
(1) it prepares photochromic colorant: surfactant sodium dodecyl base being added into aluminium chloride and neodymium chloride mixed solution
Oxalic acid solution is added dropwise later under water bath condition in sodium sulphate while stirring, then adjusts solution ph to 8~10, persistently stirs 20
~40min obtains the solution for having a large amount of pale pink precipitatings, will obtain light-induced variable after solution ultrasound, washing, suction filtration, dry, calcining
Color colorant；
(2) it prepares photochromic ceramic ink: light-induced variable will be obtained after the photochromic colorant ball milling of step (1) preparation gained
Solvent, dispersing agent and water are added into gained powder for toner material, continue ball milling mixing and obtain suspension, then surpass suspension
Sound is uniformly dispersed to obtain photochromic ceramic ink.
In above scheme, ω (neodymium chloride): ω (aluminium chloride)=1:1.3~1 in mixed solution described in step (1):
1.5。
In above scheme, the additive amount of lauryl sodium sulfate described in step (1) is that aluminium chloride and neodymium chloride mixing are molten
The 0.18~0.22% of liquid gross mass.
In above scheme, the concentration of aluminium chloride described in step (1) and neodymium chloride mixed solution is 0.05~0.15g/mL,
The concentration of the oxalic acid solution is 0.05~0.15g/mL.
In above scheme, the temperature of water-bath described in step (1) is 60~80 DEG C, the frequency of the ultrasound for 60~
80KHz, ultrasonic time are 20~40min.
In above scheme, the temperature of the calcining is 900 DEG C~1000 DEG C, and calcination time is 7.5~9.5h, the drying
Temperature be 70 DEG C~90 DEG C, drying time be 5~10h.
In above scheme, solvent described in step (2) is the mixed solution of propylene glycol and diethylene glycol (DEG), the propylene glycol and two
The mass ratio of glycol is 1:3~3:1.
In above scheme, dispersing agent described in step (2) is polyethylene glycol, polyvinyl alcohol 1750 and lauryl sodium sulfate
One or more of.
In above scheme, photochromic powder, solvent, dispersing agent and water press quality hundred in suspension described in step (2)
Divide than being calculated as: photochromic powder 30~40%, solvent 5~20%, dispersing agent 0.2~0.8%, water 39.2~64.8%.
In above scheme, the time of ball milling mixing described in step (2) is 2~4 hours, the frequency of the ultrasonic disperse
Rate is 60~80KHz, and the time of ultrasonic disperse is 30~60min.
After tested, it is 179~301nm that the present invention, which prepares the photochromic colorant powder average grain size of gained,；With the light
The ceramic ink uniform particle sizes of mutagens color colorant preparation, average grain diameter are less than 500nm, and specific gravity is 1.15~1.25, and pH value is
Viscosity is 0~10mPas at 6.90~7.10,40 DEG C, and after standing 7 days, for ceramic ink without layering and sedimentation, stability is good, symbol
Build the requirement for building ceramic ink jet printing ink jointly.
Beneficial effects of the present invention are as follows:
(1) prepare colorant low energy consumption: the present invention obtains light-induced variable through 900~1000 DEG C of calcinings using chemical coprecipitation
Color colorant, 100 DEG C lower than the firing temperature of general solid-phase synthesis or more, therefore energy saving is more than 10%；
(2) ceramic ink photochromic effect is good: photochromic ceramic ink of the invention is in light wave 200~800nm model
Enclose it is interior there are multiple reflection peaks (attached drawings 1), different colors can be presented under different light sources, photochromic effect is more preferable；
(3) ceramic ink stability is good: the present invention, as solvent, makes colorant powder form surface using water soluble organic substance
Package, it is not easy to reunite, guarantee that ceramic ink is evenly dispersed, average grain diameter is less than 500nm (attached drawing 2), after standing 7 days, no layering
And sedimentation, it avoids ceramic ink from blocking spray head in use, meets architectural pottery inkjet printing requirement.
Detailed description of the invention
Fig. 1 is reflectance spectrum figure of the photochromic ink prepared by the embodiment of the present invention 1 in visible light wave range.
Fig. 2 is the grading curve of photochromic ceramic ink prepared by the embodiment of the present invention 1.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
The preparation method of the photochromic ceramic ink of inkjet printing, including following two steps:
(1) it prepares photochromic colorant: being 0.05g/mL, ω (neodymium chloride): ω (aluminium chloride)=1:1.3 chlorine to concentration
Change the Surfactant SDS for being added in aluminium and neodymium chloride mixed solution and accounting for mixed solution gross mass 0.18%, it
The oxalic acid solution that concentration is 0.15g/mL is added dropwise under 60 DEG C of water-baths afterwards, is adjusted with the sodium hydroxide solution of concentration 1.0mol/mL
Solution ph is added dropwise simultaneously to 10, is persistently stirred with the mixing speed of 700r/min, after being added dropwise to complete, then persistently stirred
40min obtains the solution for having a large amount of pale pink precipitatings, by precipitating liquid ultrasonic (frequency 70KHz, time 20min), washing, takes out
Filter, and at 90 DEG C after dry 5h, 9h, which is calcined, at 1000 DEG C obtains photochromic colorant；
(2) it prepares photochromic ceramic ink: the photochromic colorant ball milling 3h of step (1) preparation gained is obtained into powder,
The propylene glycol and diethylene glycol (DEG) mixed solution and dispersing agent polyethylene glycol and water that mass ratio is 1:3 are added into gained powder, after
Continuous ball milling mixing 2h obtains suspension, the mass percent of each substance in suspension are as follows: photochromic powder 30%, solvent
15%, dispersing agent 0.2%, water 54.8% is then ultrasonic (frequency 80KHz, time 30min) by suspension, obtains uniform light
Mutagens color ceramic ink.
After tested, the photochromic colorant powder average grain size of the present embodiment step (1) preparation gained is 179nm；With
The photochromic ceramic ink uniform particle sizes (see Fig. 2 grading curve figure) of colorant preparation, average grain diameter are less than 500nm,
Specific gravity is 1.15, and viscosity is 2.15mPas at 6.90,40 DEG C of pH value, and after standing 7 days, ceramic ink is without layering and settles,
Stability is good, meets the requirement of architectural pottery ink jet ink for printing, and prepared photochromic ceramic ink is in light wave 200
There are multiple reflection peaks (reflectance spectrum figure of visible light wave range is shown in Fig. 1) within the scope of~800nm, can be presented under different light sources
Different colors, photochromic effect are very good.
Embodiment 2
The preparation method of the photochromic ceramic ink of inkjet printing, including following two steps:
(1) it prepares photochromic colorant: being 0.15g/mL, ω (neodymium chloride): ω (aluminium chloride)=1:1.5 chlorine to concentration
Change the Surfactant SDS for being added in aluminium and neodymium chloride mixed solution and accounting for mixed solution gross mass 0.22%, it
The oxalic acid solution that concentration is 0.05g/mL is added dropwise under 60 DEG C of water-baths afterwards, is adjusted with the sodium hydroxide solution of concentration 0.4mol/mL
Solution ph is added dropwise simultaneously, is persistently stirred with the mixing speed of 400r/min, after being added dropwise to complete, then persistently stir 20min to 8,
The solution for there are a large amount of pale pink precipitatings is obtained, by precipitating liquid ultrasonic (frequency 60KHz, time 40min), washing, is filtered, and
At 70 DEG C after dry 10h, 7.5h is calcined at 900 DEG C and obtains photochromic colorant；
(2) it prepares photochromic ceramic ink: photochromic colorant ball milling 6h obtained by step (1) being obtained into powder, to institute
It obtains and the propylene glycol that mass ratio is 3:1 and the polyethylene glycol and ten that diethylene glycol (DEG) mixed solution and mass ratio are 1:1 is added in powder
Sodium dialkyl sulfate dispersing agent, Yi Jishui continue ball milling mixing 2h and obtain suspension, the mass percent of each substance in suspension
Are as follows: photochromic powder 40%, solvent 20%, dispersing agent 0.8%, water 39.2%, then by suspension ultrasound (frequency 75KHz,
Time 60min), obtain uniform photochromic ceramic ink.
After tested, the photochromic colorant powder average grain size of the present embodiment step (1) preparation gained is 301nm；With
The colorant preparation photochromic ceramic ink uniform particle sizes, average grain diameter be less than 500nm, specific gravity 1.25, pH value 7.10,
Viscosity is 10mPas at 40 DEG C, and after standing 7 days, for ceramic ink without layering and sedimentation, stability is good, meets architectural pottery ink-jet
The requirement of ink for printing.
Embodiment 3
The preparation method of the photochromic ceramic ink of inkjet printing, including following two steps:
(1) it prepares photochromic colorant: being 0.13g/mL, ω (neodymium chloride): ω (aluminium chloride)=1:1.4 chlorine to concentration
Change the Surfactant SDS for being added in aluminium and neodymium chloride mixed solution and accounting for mixed solution gross mass 0.19%, it
The oxalic acid solution that concentration is 0.12g/mL is added dropwise under 75 DEG C of water-baths afterwards, is adjusted with the sodium hydroxide solution of concentration 0.6mol/mL
Solution ph is added dropwise simultaneously, is persistently stirred with the mixing speed of 500r/min, after being added dropwise to complete, then persistently stir 30min to 9,
The solution for there are a large amount of pale pink precipitatings is obtained, by precipitating liquid ultrasonic (frequency 80KHz, time 30min), washing, is filtered, and
At 80 DEG C after dry 10h, 8.5h is calcined at 1000 DEG C and obtains photochromic colorant；
(2) it prepares photochromic ceramic ink: photochromic colorant ball milling 5h obtained by step (1) being obtained into powder, to institute
It obtains and the propylene glycol that mass ratio is 2:1 and the polyethylene glycol that diethylene glycol (DEG) mixed solution and mass ratio are 1:1:2 is added in powder, gathers
Vinyl alcohol 1750 and lauryl sodium sulfate dispersing agent, Yi Jishui continue ball milling mixing 2h and obtain suspension, each object in suspension
The mass percent of matter are as follows: photochromic powder 35%, solvent 18%, dispersing agent 0.6%, water 46.4%, then by suspension
Ultrasonic (frequency 65KHz, time 50min) obtains uniform photochromic ceramic ink.
After tested, the photochromic colorant powder average grain size of the present embodiment step (1) preparation gained is 215nm；With
The ceramic ink uniform particle sizes of colorant preparation, average grain diameter are less than 500nm, and specific gravity 1.23 glues at 7.04,40 DEG C of pH value
Degree is 7mPas, and after standing 7 days, for ceramic ink without layering and sedimentation, stability is good, meets architectural pottery ink-jet ink
The requirement of water.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and is not the limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection scope of the invention.
Claims (10)
1. a kind of inkjet printing preparation method of photochromic ceramic ink, which comprises the steps of:
(1) it prepares photochromic colorant: surfactant sodium dodecyl base sulfuric acid being added into aluminium chloride and neodymium chloride mixed solution
Oxalic acid solution is added dropwise later under water bath condition in sodium while stirring, then adjusts solution ph to 8 ~ 10, persistently stir 20 ~
40min obtains the solution for having a large amount of pale pink precipitatings, will obtain after solution ultrasound, washing, suction filtration, dry, calcining photochromic
Colorant；
(2) it prepares photochromic ceramic ink: photochromic powder will be obtained after the photochromic colorant ball milling of step (1) preparation gained
Solvent, dispersing agent and water are added into gained powder for material, continue ball milling mixing and obtain suspension, then by suspension ultrasound point
It dissipates and uniformly obtains photochromic ceramic ink.
2. preparation method according to claim 1, which is characterized in that ω (chlorination in mixed solution described in step (1)
Neodymium): ω (aluminium chloride)=1:1.3 ~ 1:1.5.
3. preparation method according to claim 1, which is characterized in that lauryl sodium sulfate described in step (1) adds
Dosage is the 0.18 ~ 0.22% of aluminium chloride and neodymium chloride mixed solution gross mass.
4. preparation method according to claim 1, which is characterized in that aluminium chloride described in step (1) and neodymium chloride mixing
The concentration of solution is 0.05 ~ 0.15g/mL, and the concentration of the oxalic acid solution is 0.05 ~ 0.15g/mL.
5. preparation method according to claim 1, which is characterized in that the temperature of water-bath described in step (1) is 60 ~ 80
DEG C, the frequency of the ultrasound is 60 ~ 80KHz, and ultrasonic time is 20 ~ 40min.
6. preparation method according to claim 1, which is characterized in that the temperature of the calcining is 900 DEG C ~ 1000 DEG C, is forged
The burning time is 7.5 ~ 9.5h, and the temperature of the drying is 70 DEG C ~ 90 DEG C, and drying time is 5 ~ 10h.
7. preparation method according to claim 1, which is characterized in that solvent described in step (2) is that propylene glycol and two are sweet
The mass ratio of the mixed solution of alcohol, the propylene glycol and diethylene glycol (DEG) is 1:3 ~ 3:1.
8. preparation method according to claim 1, which is characterized in that dispersing agent described in step (2) is polyethylene glycol, gathers
One or more of vinyl alcohol 1750 and lauryl sodium sulfate.
9. preparation method according to claim 1, which is characterized in that photochromic powder in suspension described in step (2)
Material, solvent, dispersing agent and water are by mass percentage are as follows: photochromic powder 30 ~ 40%, solvent 5 ~ 20%, dispersing agent 0.2 ~
0.8%, water 39.2 ~ 64.8%.
10. preparation method according to claim 1, which is characterized in that the time of ball milling mixing described in step (2) be 2 ~
4 hours, the frequency of the ultrasonic disperse was 60 ~ 80KHz, and the time of ultrasonic disperse is 30 ~ 60min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112409846A (en) * | 2020-11-24 | 2021-02-26 | 陕西科技大学 | Photochromic ink-jet printable aqueous fluorescent ink and preparation method thereof |
| CN112876901A (en) * | 2021-02-07 | 2021-06-01 | 中北大学 | Water-dispersible functional ceramic ink and preparation and application thereof |
| CN114958188A (en) * | 2022-05-31 | 2022-08-30 | 书香门地集团股份有限公司 | Thermochromic water-based UV coating and preparation method thereof |
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Cited By (5)
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| CN112409846A (en) * | 2020-11-24 | 2021-02-26 | 陕西科技大学 | Photochromic ink-jet printable aqueous fluorescent ink and preparation method thereof |
| CN112876901A (en) * | 2021-02-07 | 2021-06-01 | 中北大学 | Water-dispersible functional ceramic ink and preparation and application thereof |
| CN112876901B (en) * | 2021-02-07 | 2022-11-15 | 中北大学 | Water-dispersible functional ceramic ink and preparation and application thereof |
| CN114958188A (en) * | 2022-05-31 | 2022-08-30 | 书香门地集团股份有限公司 | Thermochromic water-based UV coating and preparation method thereof |
| CN114958188B (en) * | 2022-05-31 | 2023-06-06 | 书香门地集团股份有限公司 | Thermochromic water-based UV paint and preparation method thereof |
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