CN105368132A - Noctilucent printing ink and preparation method thereof - Google Patents
Noctilucent printing ink and preparation method thereof Download PDFInfo
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- CN105368132A CN105368132A CN201510948881.4A CN201510948881A CN105368132A CN 105368132 A CN105368132 A CN 105368132A CN 201510948881 A CN201510948881 A CN 201510948881A CN 105368132 A CN105368132 A CN 105368132A
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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
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
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Abstract
The invention discloses noctilucent printing ink and a preparation method thereof. The noctilucent printing ink is prepared from, by weight, 20-30 parts of graphene/filler mixed material, 1-5 parts of graphene/red-emit phosphor/SiO2 composite material, 1-5 parts of graphene/long afterglow phosphor composite material, 40-50 parts of organic resin, 5-20 parts of organic solvent, 0.5-5 parts of dispersing agent and 0.5-3 parts of anti-settling agent. The printing ink has the characteristics of being high in quality and good in property. By the adoption of the preparation method, the luminous intensity of the luminous printing ink can be enhanced obviously, the luminous uniformity of the luminous printing ink can be improved remarkably, and the afterglow time of the luminous printing ink can be prolonged prominently; meanwhile, the dispersity of the phosphor in the printing ink is improved, and the construction performance and storage stability of the printing ink are also improved.
Description
Technical field
The present invention relates to a kind of luminescent ink and preparation method thereof.
Background technology
Along with the development that China's economic construction and printing technology are advanced by leaps and bounds, Printing ink producing is all improved in quantity, kind and quality.China's ink output accounts for 6% of world's ink ultimate production, has become the fourth-largest Printing ink producing state of the world.Raw-material price increase impels ink enterprise to reduce costs to make larger effort.The a little filler of suitable employing, both can reduce amount of pigment, reduce costs, again the character of adjustable ink, as rare thick, mobility etc., also improved the handiness of formulating of recipe.
But the fillers dispersed of adding in current ink preparation technology is poor, when need enter next step grinding step, needing to increase grinding number of times could control the fineness watering down ink in acceptability limit, thus causes Printing ink producing efficiency low, and cost is high; The decline of the ink quality such as glossiness, mobility of ink can be there is simultaneously, had a strong impact on the performance of ink.When adding fluorescent material to ink, due to the bad dispersibility of fluorescent material in ink, easily there is agglomeration, precipitation, layering can be caused, uniformity of luminance is poor, causes ink workability, poor storage stability and poor adhesive force, and luminescent properties and/or twilight sunset effect also can be lost seriously.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the invention provides a kind of luminescent ink and preparation method thereof, this ink has the characteristic that quality is high, ink performance is good, this preparation method can significantly improve the luminous intensity of luminous printing ink, uniformity of luminance, time of persistence, improves the dispersiveness of fluorescent material in ink, ink workability and stability in storage simultaneously.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of luminescent ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 20 ~ 30 parts, Graphene/red light fluorescent powder/SiO
21 ~ 5 part, matrix material, Graphene/long-afterglow fluorescent powder composite material 1 ~ 5 part, organic resin 40 ~ 50 parts, organic solvent 5 ~ 20 parts, dispersion agent 0.5 ~ 5 part, anti-settling agent 0.5 ~ 3 part.
A preparation method for luminescent ink, comprises the following steps:
(1) Graphene/long-afterglow fluorescent powder composite material is prepared: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; 25 ~ 100g long persistence luminescent powder is added in 500ml deionized water, obtained long persistence luminescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; Down in graphene dispersing solution, slowly drip long persistence luminescent powder dispersion liquid 100kW is ultrasonic, ultrasonic 30 ~ 60min, then suction filtration, oven dry, carry out 1050 DEG C of thermal treatment 30min under vacuum environment, thermal treatment 60min at 1250 DEG C again, obtained Graphene/long-afterglow fluorescent powder composite material;
(2) by 10 ~ 20 parts of Graphene/kaolin/SiO
2compounded mix and 5 ~ 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 ~ 20 parts of deionized waters under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, and process 90 ~ 120min forms solution A 3; By 1 ~ 5 part of Graphene/red light fluorescent powder/SiO
2matrix material is scattered in 15 ~ 20 parts of deionized waters under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, and process 90 ~ 120min forms solution B 3; Be scattered in 15 ~ 20 parts of deionized waters by 1 ~ 5 part of Graphene/long-afterglow fluorescent powder composite material under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, process 90 ~ 120min forms solution C 1; Under 200 ~ 400KW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir, slowly dropping solution B 3, C1 form mixing solutions to solution A 3 respectively; Organic resin 40 ~ 50 parts, organic solvent 5 ~ 20 parts are put into container, adds dispersion agent 0.5 ~ 5 part, stir, under whipped state, add anti-settling agent 0.5 ~ 3 part, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
In the present invention, described organic resin is one or several in epoxy resin, urethane resin, amino varnish, vibrin, acrylic resin, Hydroxylated acrylic resin, acroleic acid polyurethane varnish, the alkyd varnish of color and luster money, fluoro-resin, and the present invention is preferably Hydroxylated acrylic resin.
Described organic solvent is one or several in ethanol, propylene glycol monomethyl ether, diethylene glycol monobutyl ether, dimethyl ether.The present invention is preferably ethanol.
Described dispersion agent is one or several in methyl-silicone oil xylene soluble liquid, homopolymer, oxidized homopolymer, ethylene acrylic acid co polymer, ethylene vinyl acetate multipolymer, low molecule ionomer.The present invention is preferably ethylene acrylic acid co polymer.
Described anti-settling agent is one or several in the N-Methyl pyrrolidone solution of aerosil, polyolefin-wax particulate, polyamide wax, modified polyurea.The present invention is preferably polyamide wax.
The present invention has following beneficial effect: the preparation method of this luminescent ink can significantly improve the luminous intensity of water-based luminous printing ink, luminescence all even time of persistence, improve the dispersiveness of fluorescent material in ink, ink workability and stability in storage simultaneously, there is good economic benefit.
Embodiment
In the present invention,
(1) Graphene is obtained by following methods: get a certain amount of sour flat band ink, 1000 DEG C process 1 hour, then at 7%H in atmosphere
2nitrogen and hydrogen mixture in 1000 DEG C of in-situ reducing process 1.5 hours, add the macrogol ester of mass ratio 3% and tetracarboxylic dianhydride's dinaphthyl of mass ratio 5.0% again, the slurry that concentration is 80.0% is made into water, first under power is the ultrasonic assistant of 400W, carry out 3500 turns/min ball milling 8 hours, 2000 turns/min ball milling is carried out 4 hours under being adjusted to 200W ultrasonic wave again, be separated through supercentrifuge 10000 turns/min after ball milling, lyophilize, obtain Graphene solid.
(2) quantum dot calcium carbonate, its preparation method can prepare the method for nano calcium carbonate quantum dot with reference to a kind of microemulsion system disclosed in Chinese patent CN103570051B, specifically first prepare the nano-calcium carbonate microemulsion of 1 ~ 3nm, then through rotary evaporation also dry obtained quantum dot calcium carbonate powders.
(3) preparation method of nano-kaoline is as follows: by 150g kaolin ore with the rotating speed ball milling 60min of 1500 turns/min, then insert in 5L deionized water, add 220g Potassium ethanoate and stir 60min, suction filtration cleaning is about 7 to pH value, then with the rotating speed ball milling 60min of 1200 turns/min after drying under 80 degree of conditions, carry out 1800 turns/min ball milling under being adjusted to 300W ultrasonic wave again 1 hour, obtain the kaolin powder of particle diameter at 10 ~ 30nm.
(4) Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano fluorescent powder, preparation method thereof is as follows: (a) is by 2.4mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 10ml ethylene glycol and 3ml distilled water; B above-mentioned solution 300r/min centrifugal speed is stirred below the dropwise Y (NO of instillation containing the certain proportioning of 2.7mmol by ()
3)
36H
2o, Eu (NO
3)
3, Al (NO
3)
3(0.9:0.04:0.06) in 12ml ethylene glycol solution, then clarify to solution at 500r/min centrifugal speed stirring 5 ~ 10min, add 15ml distilled water; C reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml by (), under vacuum conditions, and 170
oinsulation reaction 90min under C, after reaction terminates, is quickly cooled to room temperature; Gained suspension is poured out, centrifugal and obtain white precipitates by acetone and washed with de-ionized water 3 times successively; D this is deposited in 90 by ()
ounder C, dry 4h, obtains nano-phosphor; E nano-phosphor ultrasonic agitation (300 ~ 500KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir) is scattered in ethanol by (); Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nano-phosphor after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 6 hours; Carry out centrifugal and obtain white precipitate 3 times by acetone and washed with de-ionized water successively; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2core-shell nano fluorescent material; F this is coated with SiO by ()
2core-shell nano fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; G fluorescent material mixture is immersed in ultrasonic 1h in hydrofluoric acid by (), remove silicon-dioxide, centrifugal and dry, obtains the Y of median size 10 ~ 20nm
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor.
(5) graphene/carbon acid calcium compounded mix, Graphene/kaolin compounded mix, Graphene/red light fluorescent powder matrix material, Graphene/long-afterglow fluorescent powder composite material is prepared:
The preparation method of graphene/carbon acid calcium compounded mix is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 1000r/min centrifugal speed stir; 100g quantum dot calcium carbonate is added in 500ml deionized water, obtained calcium carbonate dispersion liquid after dispersion 240 ~ 300min under 1200 ~ 1500kW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir; In graphene dispersing solution, slowly drip calcium carbonate dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained graphene/carbon acid calcium compounded mix down 100kW is ultrasonic.
The preparation method of Graphene/kaolin compounded mix is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; 50g nano kaoline is added in 500ml deionized water, obtained Dispersion of Kaolin liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; In graphene dispersing solution, slowly drip Dispersion of Kaolin liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/kaolin compounded mix down 100kW is ultrasonic.
The preparation method of Graphene/red light fluorescent powder matrix material is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; By 25 ~ 100gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; In graphene dispersing solution, slowly drip red light fluorescent powder dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic.
The preparation method of Graphene/long-afterglow fluorescent powder composite material is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; 25 ~ 100g long persistence luminescent powder is added in 500ml deionized water, obtained long persistence luminescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; Down in graphene dispersing solution, slowly drip long persistence luminescent powder dispersion liquid 100kW is ultrasonic, ultrasonic 30 ~ 60min, then suction filtration, oven dry, carry out 1050 DEG C of thermal treatment 30min under vacuum environment, thermal treatment 60min at 1250 DEG C again, obtained Graphene/long-afterglow fluorescent powder composite material.Described long persistence luminescent powder is steady persistence Sr
4al
14o
25nano-phosphor.
(6) graphene/carbon acid calcium/SiO is prepared
2compounded mix, Graphene/kaolin/SiO
2compounded mix, Graphene/red light fluorescent powder/SiO
2matrix material, Graphene/long persistence luminescent powder/SiO
2matrix material:
Graphene/carbon acid calcium/SiO
2compounded mix preparation method is as follows: be scattered in ethanol by graphene/carbon acid calcium compounded mix ultrasonic agitation (400KW ultrasonic vibration and 1000r/min centrifugal speed stir); Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and graphene/carbon acid calcium compounded mix after stirring is 1.8:1, adjust ph is 9, temperature of reaction is 25 DEG C, react 5 hours, carry out centrifugal and obtain precipitation 3 times by acetone and deionized water, washed with de-ionized water successively; This is deposited in 90
odry 2h under C, to obtain being coated with SiO
2graphene/carbon acid calcium/SiO
2compounded mix.
Graphene/kaolin/SiO
2compounded mix preparation method is as follows: be scattered in ethanol by Graphene/kaolin compounded mix ultrasonic agitation (400KW ultrasonic vibration and 1000r/min centrifugal speed stir); Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/kaolin compounded mix after stirring is 1.8:1, adjust ph is 9, temperature of reaction is 25 DEG C, react 5 hours, carry out centrifugal and obtain precipitation 3 times by acetone and deionized water, washed with de-ionized water successively; This is deposited in 90
odry 2h under C, to obtain being coated with SiO
2graphene/kaolin/SiO
2compounded mix.
Graphene/red light fluorescent powder/SiO
2the preparation method of matrix material is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; By 25 ~ 100gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; In graphene dispersing solution, slowly drip red light fluorescent powder dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic; 0.5g Graphene/red light fluorescent powder compound material ultrasound being stirred (300 ~ 500KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/red light fluorescent powder matrix material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; This is coated with SiO
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; This mixture is immersed in ultrasonic 5 ~ 60min in hydrofluoric acid, removes the silicon-dioxide of part, centrifugal and dry, obtain Graphene/Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06fluorescent material/SiO
2matrix material.
Graphene/long persistence luminescent powder/SiO
2the preparation method of matrix material is as follows: 1g Graphene adds in 100ml deionized water by (a), obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; B 25 ~ 100g long persistence luminescent powder adds in 500ml deionized water by (), obtained long persistence luminescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; C () slowly drips long persistence luminescent powder dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/long-afterglow fluorescent powder composite material down 100kW is ultrasonic in graphene dispersing solution; D 0.5g Graphene/long persistence luminescent powder compound material ultrasound stirs by () (300 ~ 500KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/long-afterglow fluorescent powder composite material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; E this is deposited in 90 by ()
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; F this is coated with SiO by ()
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; G this mixture is immersed in ultrasonic 5 ~ 60min in hydrofluoric acid by (), remove the silicon-dioxide of part, centrifugal and dry, obtains Graphene/long persistence luminescent powder/SiO
2matrix material.
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention, is not limitation of the invention.
Embodiment 1
A kind of ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:1.
A kind of ink preparation method, comprises the following steps:
(1) Graphene, quantum dot calcium carbonate and kaolin powder is prepared;
(2) graphene/carbon acid calcium compounded mix and Graphene/kaolin compounded mix is prepared;
(3) Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix are mixed into Graphene/filler mixing material by weight 3:1; Organic resin, organic solvent are put into container, adds dispersion agent, carry out 12 stirrings, under whipped state, add anti-settling agent, Graphene/filler mixing material successively; Improve rotating speed after adding Graphene/filler mixing material, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained ink.
The glossiness of this ink and good flowing properties, application property, stability in storage are good.
Embodiment 2
A kind of ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A kind of ink preparation method, comprises the following steps:
(1) Graphene, quantum dot calcium carbonate and kaolin powder is prepared;
(2) graphene/carbon acid calcium compounded mix and Graphene/kaolin compounded mix is prepared;
(3) Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix are mixed into Graphene/filler mixing material by weight 3:2; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, Graphene/filler mixing material successively; Improve rotating speed after adding Graphene/filler mixing material, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained ink.
Better, application property, stability in storage are better for the glossiness of this ink and flowing property.
Embodiment 3
A kind of ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 30 parts, organic resin 45 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A kind of ink preparation method, comprises the following steps:
(1) Graphene, quantum dot calcium carbonate and kaolin powder is prepared;
(2) graphene/carbon acid calcium compounded mix and Graphene/kaolin compounded mix is prepared;
(3) Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix are mixed into Graphene/filler mixing material by weight 3:2; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, Graphene/filler mixing material successively; Improve rotating speed after adding Graphene/filler mixing material, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained ink.
Better, application property, stability in storage are better for the glossiness of this ink and flowing property.
Embodiment 4
A kind of ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 1:2.
A kind of ink preparation method, comprises the following steps:
(1) Graphene, quantum dot calcium carbonate and kaolin powder is prepared;
(2) graphene/carbon acid calcium compounded mix and Graphene/kaolin compounded mix is prepared;
(3) Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix are mixed into Graphene/filler mixing material by weight 1:2; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, Graphene/filler mixing material successively; Improve rotating speed after adding Graphene/filler mixing material, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained ink.
The glossiness of this ink and good flowing properties, application property, stability in storage are good.
Embodiment 5
A kind of ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is Graphene/kaolin compounded mix, graphene/carbon acid calcium compounded mix and Graphene mix by weight 3:2:2.
A kind of ink preparation method, comprises the following steps:
(1) Graphene, quantum dot calcium carbonate and kaolin powder is prepared;
(2) graphene/carbon acid calcium compounded mix and Graphene/kaolin compounded mix is prepared;
(3) Graphene/kaolin compounded mix, graphene/carbon acid calcium compounded mix and Graphene are mixed into Graphene/filler mixing material by weight 3:2:2; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, Graphene/filler mixing material successively; Improve rotating speed after adding Graphene/filler mixing material, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained ink.
Glossiness and the flowing property of this ink are excellent, and application property, stability in storage are excellent.
Comparative example 1
Based on the preparation technology of embodiment 1, made into by Graphene/filler mixing material separately to add Graphene and filler, filler is at least one such as calcium carbonate, kaolin; All the other are identical with embodiment 1, obtained ink, and generally, application property, stability in storage are general for its glossiness and flowing property.
Comparative example 2
Based on the preparation technology of embodiment 1, do not add Graphene/filler mixing material, obtained ink, its glossiness and poor mobile performance, application property, poor storage stability.
Comparative example 3
Based on the preparation technology of embodiment 1, changed into and only add filler by Graphene/filler mixing material, filler is at least one such as calcium carbonate, kaolin; All the other are identical with embodiment 2, obtained ink, its glossiness and flowing property poor, application property, stability in storage are poor.
Embodiment 6
A kind of luminous printing ink, it is made up of the raw material of following weight part: Graphene/5 parts, red light fluorescent powder matrix material, Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A preparation method for luminous printing ink, it comprises the following steps:
(1) Graphene/red light fluorescent powder matrix material is prepared: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution disperse 180min under 800kW ultrasonic vibration and 800r/min centrifugal speed stir after; By 25gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid disperse 240min under 1000kW ultrasonic vibration and 800r/min centrifugal speed stir after; In graphene dispersing solution, slowly drip red light fluorescent powder dispersion liquid, ultrasonic 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic;
(2) by 15 parts of Graphene/kaolin/SiO
2compounded mix and 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution A 1; Be scattered in 15 parts of deionized waters by 5 parts of Graphenes/red light fluorescent powder matrix material under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, process 100min forms solution B 1; Under 400KW ultrasonic vibration and 800r/min centrifugal speed stir, slowly drip in solution B 1 to solution A 1 and form mixing solutions; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and good flowing properties, application property, stability in storage are good, fluorescent material good dispersity, evenly luminous, and intensity is good.
Embodiment 7
Based on the preparation method of embodiment 6, by the Y in step (1)
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor addition is revised as 50g, and all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and fluorescent material is better dispersed, luminous even, and intensity is better.
Embodiment 8
Based on the preparation method of embodiment 6, by the Y in step (1)
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor addition is revised as 100g, and all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and good flowing properties, application property, stability in storage are good, fluorescent material good dispersity, evenly luminous, and intensity is good.
Embodiment 9
Based on the preparation method of embodiment 6, add 1 part of Graphene in the mixing solutions in step (2), all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and flowing property excellent, application property, stability in storage are excellent, wear resistant high-adhesion, fluorescent material good dispersity, evenly luminous, and intensity is good.
Comparative example 4
A kind of luminous printing ink, it is made up of the raw material of following weight part: 5 parts, red light fluorescent powder matrix material, Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A preparation method for luminous printing ink, it comprises the following steps: by 15 parts of Graphene/kaolin/SiO
2compounded mix and 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution A; By 5 parts of Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution B; Under 400KW ultrasonic vibration and 800r/min centrifugal speed stir, slowly drip in solution B to solution A and form mixing solutions; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and good flowing properties, application property, stability in storage are good, and fluorescent material is dispersed general, and uniformity of luminance is general, and intensity is general.
Comparative example 5
Based on the preparation method of embodiment 6, the solution A 1 in step (2) removed, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and poor mobile performance, application property, poor storage stability, fluorescent material bad dispersibility, luminescence is evenly poor, and intensity is general.
Comparative example 6
Based on the preparation method of embodiment 6, step (1) is revised as:
A () is by 2.4mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 10ml ethylene glycol and 3ml distilled water; B above-mentioned solution 300r/min centrifugal speed is stirred below the dropwise Y (NO of instillation containing the certain proportioning of 2.7mmol by ()
3)
36H
2o, Eu (NO
3)
3, Al (NO
3)
3(0.9:0.04:0.06) in 12ml ethylene glycol solution, then clarify to solution at 500r/min centrifugal speed stirring 5 ~ 10min, add the distilled water of 15ml containing 0.01g Graphene; C reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml by (), under vacuum conditions, and 170
oinsulation reaction 90min under C, after reaction terminates, is quickly cooled to room temperature; Gained suspension is poured out, centrifugal and obtain precipitation by acetone and washed with de-ionized water 3 times successively; D this is deposited in 90 by ()
odry 4h under C, obtains graphene/nanometer fluorescent material matrix material; E graphene/nanometer fluorescent material compound material ultrasound stirs by () (500KW ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and graphene/nanometer fluorescent material matrix material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 6 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; F this is coated with SiO by ()
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain mixture; G this mixture is immersed in ultrasonic 1h in hydrofluoric acid by (), remove silicon-dioxide, centrifugal and dry, obtains Graphene/Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06fluorescent material matrix material.
All the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, its glossiness and good flowing properties, application property, stability in storage are good, and fluorescent material is dispersed general, and uniformity of luminance is general, and intensity is general.
Embodiment 10
A kind of luminous printing ink, it is made up of the raw material of following weight part: Graphene/red light fluorescent powder/SiO
25 parts, matrix material, Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A preparation method for luminous printing ink, it comprises the following steps:
(1) Graphene/red light fluorescent powder/SiO is prepared
2matrix material: 1g Graphene adds in 100ml deionized water by (a), obtained graphene dispersing solution disperse 180min under 800kW ultrasonic vibration and 800r/min centrifugal speed stir after; B () is by 25gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid disperse 240min under 1000kW ultrasonic vibration and 800r/min centrifugal speed stir after; C () slowly drips red light fluorescent powder dispersion liquid, ultrasonic 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic in graphene dispersing solution; D 0.5g Graphene/red light fluorescent powder compound material ultrasound stirs by () (300KW ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/red light fluorescent powder matrix material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; E this is deposited in 90 by ()
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; F this is coated with SiO by ()
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; G this mixture is immersed in ultrasonic 5min in hydrofluoric acid by (), remove the silicon-dioxide of part, centrifugal and dry, obtains Graphene/Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06fluorescent material/SiO
2matrix material.
(2) by 15 parts of Graphene/kaolin/SiO
2compounded mix and 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution A 2; By 5 parts of Graphene/red light fluorescent powder/SiO
2matrix material is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution B 2; Under 400KW ultrasonic vibration and 800r/min centrifugal speed stir, slowly drip in solution B 2 to solution A 2 and form mixing solutions; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, and fluorescent material dispersiveness is excellent, and uniformity of luminance is excellent, and intensity is better for its glossiness and flowing property.
Embodiment 11
Based on the preparation method of embodiment 10, mixture in step (1) is immersed in ultrasonic time in hydrofluoric acid and is revised as 30min, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, and fluorescent material dispersiveness is more excellent, and uniformity of luminance is more excellent, and intensity is excellent for its glossiness and flowing property.
Embodiment 12
Based on the preparation method of embodiment 10, mixture in step (1) is immersed in ultrasonic time in hydrofluoric acid and is revised as 60min, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, and fluorescent material dispersiveness is excellent, and uniformity of luminance is excellent, and intensity is better for its glossiness and flowing property.
Comparative example 7
Based on the preparation method of embodiment 12, remove in step (1) and this is coated with SiO
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h; All the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and fluorescent material is dispersed general, and uniformity of luminance is general, and intensity is general.
Embodiment 13
A kind of luminous printing ink, it is made up of the raw material of following weight part: Graphene/red light fluorescent powder/SiO
25 parts, matrix material, Graphene/long-afterglow fluorescent powder composite material 5 parts, Graphene/filler mixing material 25 parts, organic resin 50 parts, organic solvent 10 parts, dispersion agent 0.5%, anti-settling agent 0.5%; Described Graphene/filler mixing material is that Graphene/kaolin compounded mix and graphene/carbon acid calcium compounded mix mix by weight 3:2.
A preparation method for luminous printing ink, it comprises the following steps:
(1) Graphene/red light fluorescent powder/SiO is prepared
2matrix material: 1g Graphene adds in 100ml deionized water by (a), obtained graphene dispersing solution disperse 180min under 800kW ultrasonic vibration and 800r/min centrifugal speed stir after; B () is by 25gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid disperse 240min under 1000kW ultrasonic vibration and 800r/min centrifugal speed stir after; C () slowly drips red light fluorescent powder dispersion liquid, ultrasonic 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic in graphene dispersing solution; D 0.5g Graphene/red light fluorescent powder compound material ultrasound stirs by () (300KW ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/red light fluorescent powder matrix material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; E this is deposited in 90 by ()
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; F this is coated with SiO by ()
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; G this mixture is immersed in ultrasonic 5min in hydrofluoric acid by (), remove the silicon-dioxide of part, centrifugal and dry, obtains Graphene/Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06fluorescent material/SiO
2matrix material.
(2) Graphene/long-afterglow fluorescent powder composite material is prepared: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution disperse 180min under 1000kW ultrasonic vibration and 800r/min centrifugal speed stir after; 25g long persistence luminescent powder is added in 500ml deionized water, obtained long persistence luminescent powder dispersion liquid disperse 300min under 1000kW ultrasonic vibration and 800r/min centrifugal speed stir after; Down in graphene dispersing solution, slowly drip long persistence luminescent powder dispersion liquid 100kW is ultrasonic, ultrasonic 60min, then suction filtration, oven dry, carry out 1050 DEG C of thermal treatment 30min under vacuum environment, thermal treatment 60min at 1250 DEG C again, obtained Graphene/long-afterglow fluorescent powder composite material.
(3) by 15 parts of Graphene/kaolin/SiO
2compounded mix and 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution A 3; By 5 parts of Graphene/red light fluorescent powder/SiO
2matrix material is scattered in 15 parts of deionized waters under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, and process 100min forms solution B 3; Be scattered in 15 parts of deionized waters by 5 parts of Graphenes/long-afterglow fluorescent powder composite material under 500KW ultrasonic vibration and 1200r/min centrifugal speed stir, process 100min forms solution C 1; Under 400KW ultrasonic vibration and 800r/min centrifugal speed stir, slowly dropping solution B 3, C1 form mixing solutions to solution A 3 respectively; Organic resin, organic solvent are put into container, adds dispersion agent, stir, under whipped state, add anti-settling agent, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, two kinds of fluorescent material good dispersitys, and intensity is better for its glossiness and flowing property; Noctilucence sunset glow is for up to 5h, and intensity is good, and uniformity of luminance is good.
Embodiment 14
Based on the preparation method of embodiment 13, the long persistence luminescent powder addition in step (2) is revised as 50g, and all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and two kinds of fluorescent material are better dispersed, and intensity is better; Noctilucence sunset glow is for up to 10h, and intensity is better, and uniformity of luminance is better.
Embodiment 15
Based on the preparation method of embodiment 13, the long persistence luminescent powder addition in step (2) is revised as 100g, and all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, two kinds of fluorescent material good dispersitys, and intensity is better for its glossiness and flowing property; Noctilucence sunset glow is for up to 10h, and intensity is good, and uniformity of luminance is general.
Embodiment 16
Based on the preparation method of embodiment 13, add 1 part of Graphene in mixing solutions in step (3), all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better, wear resistant high-adhesion for its glossiness and flowing property; Two kinds of fluorescent material are better dispersed, and uniformity of luminance is better, and intensity is better; Noctilucence sunset glow is for up to 10h, and intensity is good, and uniformity of luminance is better.
Comparative example 8
Based on the preparation method of embodiment 13, remove step (2), in step (3) Graphene/long-afterglow fluorescent powder composite material is replaced to long persistence luminescent powder, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property; Two kinds of fluorescent material are dispersed general, and intensity is better; The noctilucence sunset glow time is short, and intensity is general, non-uniform light.
Embodiment 17
Based on the preparation method of embodiment 13, Graphene/long-afterglow fluorescent powder composite material prepared by step (2) and be revised as and prepare Graphene/long persistence luminescent powder/SiO
2matrix material, concrete preparation process: 1g Graphene adds in 100ml deionized water by (a), obtained graphene dispersing solution disperse 200min under 1000kW ultrasonic vibration and 500r/min centrifugal speed stir after; B 25g long persistence luminescent powder adds in 500ml deionized water by (), obtained long persistence luminescent powder dispersion liquid disperse 240min under 1000kW ultrasonic vibration and 1000r/min centrifugal speed stir after; C () slowly drips long persistence luminescent powder dispersion liquid down 100kW is ultrasonic in graphene dispersing solution, ultrasonic 60min, then suction filtration, oven dry, carry out 1050 DEG C of thermal treatment 30min under vacuum environment, thermal treatment 60min at 1250 DEG C again, obtained Graphene/long-afterglow fluorescent powder composite material; D 0.5g Graphene/long persistence luminescent powder compound material ultrasound stirs by () (500KW ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol; Add a certain proportion of (5:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/long-afterglow fluorescent powder composite material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; E this is deposited in 90 by ()
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; F this is coated with SiO by ()
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; G this mixture is immersed in ultrasonic 5min in hydrofluoric acid by (), remove the silicon-dioxide of part, centrifugal and dry, obtains Graphene/long persistence luminescent powder/SiO
2matrix material;
All the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and two kinds of fluorescent material are better dispersed, and intensity is better; Noctilucence sunset glow is for up to 11h, and intensity is good, and uniformity of luminance is excellent.
Embodiment 18
Based on the preparation method of embodiment 17, mixture in step (2) is immersed in ultrasonic time in hydrofluoric acid and is revised as 30min, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and two kinds of fluorescent material are better dispersed, and intensity is better; Noctilucence sunset glow is for up to 12h, and intensity is better, and uniformity of luminance is more excellent.
Embodiment 19
Based on the preparation method of embodiment 17, mixture in step (2) is immersed in ultrasonic time in hydrofluoric acid and is revised as 60min, all the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and two kinds of fluorescent material are better dispersed, and intensity is better; Noctilucence sunset glow is for up to 10.5h, and intensity is good, and uniformity of luminance is excellent.
Comparative example 9
Based on the preparation method of embodiment 19, remove in step (2) and this is coated with SiO
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h; All the other are constant, obtained luminous printing ink.
Obtained luminous printing ink, better, application property, stability in storage are better for its glossiness and flowing property, and two kinds of fluorescent material are better dispersed, and intensity is better; Noctilucence sunset glow is for up to 10h, and intensity is general, and uniformity of luminance is poor.
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (10)
1. a luminescent ink, it is made up of the raw material of following weight part: Graphene/filler mixing material 20 ~ 30 parts, Graphene/red light fluorescent powder/SiO
21 ~ 5 part, matrix material, Graphene/long-afterglow fluorescent powder composite material 1 ~ 5 part, organic resin 40 ~ 50 parts, organic solvent 5 ~ 20 parts, dispersion agent 0.5 ~ 5 part, anti-settling agent 0.5 ~ 3 part.
2. a preparation method for luminescent ink, comprises the following steps:
(1) Graphene/long-afterglow fluorescent powder composite material is prepared: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; 25 ~ 100g long persistence luminescent powder is added in 500ml deionized water, obtained long persistence luminescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; Down in graphene dispersing solution, slowly drip long persistence luminescent powder dispersion liquid 100kW is ultrasonic, ultrasonic 30 ~ 60min, then suction filtration, oven dry, carry out 1050 DEG C of thermal treatment 30min under vacuum environment, thermal treatment 60min at 1250 DEG C again, obtained Graphene/long-afterglow fluorescent powder composite material;
(2) by 10 ~ 20 parts of Graphene/kaolin/SiO
2compounded mix and 5 ~ 10 parts of graphene/carbon acid calcium/SiO
2compounded mix is scattered in 15 ~ 20 parts of deionized waters under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, and process 90 ~ 120min forms solution A 3; By 1 ~ 5 part of Graphene/red light fluorescent powder/SiO
2matrix material is scattered in 15 ~ 20 parts of deionized waters under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, and process 90 ~ 120min forms solution B 3; Be scattered in 15 ~ 20 parts of deionized waters by 1 ~ 5 part of Graphene/long-afterglow fluorescent powder composite material under 500 ~ 800KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir, process 90 ~ 120min forms solution C 1; Under 200 ~ 400KW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir, slowly dropping solution B 3, C1 form mixing solutions to solution A 3 respectively; Organic resin 40 ~ 50 parts, organic solvent 5 ~ 20 parts are put into container, adds dispersion agent 0.5 ~ 5 part, stir, under whipped state, add anti-settling agent 0.5 ~ 3 part, mixing solutions successively; Improve rotating speed after adding mixing solutions, control churning time is 30min, and whipping temp is 60 DEG C, filters i.e. obtained luminous printing ink.
3. the preparation method of luminescent ink according to claim 2, is characterized in that, described Graphene/red light fluorescent powder/SiO
2composite material and preparation method thereof is as follows: be scattered in ethanol by 0.5g Graphene/red light fluorescent powder matrix material under 300 ~ 500KW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir; Add a certain proportion of water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/red light fluorescent powder matrix material after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 12 hours; Carry out centrifugal and obtain precipitation 3 times by acetone and washed with de-ionized water successively; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2core-shell composite material; This is coated with SiO
2core-shell composite material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1.5h, obtain mixture; This mixture is immersed in ultrasonic 5 ~ 60min in hydrofluoric acid, removes the silicon-dioxide of part, centrifugal and dry, obtain Graphene/Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06fluorescent material/SiO
2matrix material.
4. the preparation method of luminescent ink according to claim 3, it is characterized in that, described Graphene/red light fluorescent powder composite material and preparation method thereof is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; By 25 ~ 100gY
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor adds in 500ml deionized water, obtained red light fluorescent powder dispersion liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; In graphene dispersing solution, slowly drip red light fluorescent powder dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/red light fluorescent powder matrix material down 100kW is ultrasonic.
5. the preparation method of luminescent ink according to claim 4, is characterized in that, described Y
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano fluorescent powder, preparation method thereof is as follows: (a) is by 2.4mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 10ml ethylene glycol and 3ml distilled water; B above-mentioned solution 300r/min centrifugal speed is stirred below the dropwise Y (NO of instillation containing the certain proportioning of 2.7mmol by ()
3)
36H
2o, Eu (NO
3)
3, Al (NO
3)
312ml ethylene glycol solution in, then 500r/min centrifugal speed stir 5 ~ 10min clarify to solution, add 15ml distilled water; C reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml by (), under vacuum conditions, and 170
oinsulation reaction 90min under C, after reaction terminates, is quickly cooled to room temperature; Gained suspension is poured out, centrifugal and obtain white precipitates by acetone and washed with de-ionized water 3 times successively; D this is deposited in 90 by ()
ounder C, dry 4h, obtains nano-phosphor; E nano-phosphor ultrasonic agitation is scattered in ethanol by (); Add a certain proportion of water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nano-phosphor after stirring is 1.8:1, and adjust ph is 9, and temperature of reaction is 25 DEG C, reacts 6 hours; Carry out centrifugal and obtain white precipitate 3 times by acetone and washed with de-ionized water successively; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2core-shell nano fluorescent material; F this is coated with SiO by ()
2core-shell nano fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain fluorescent material mixture; G fluorescent material mixture is immersed in ultrasonic 1h in hydrofluoric acid by (), remove silicon-dioxide, centrifugal and dry, obtains the Y of median size 10 ~ 20nm
0.9vO
4: Eu
3+ 0.04, Al
3+ 0.06nano-phosphor.
6. the preparation method of luminescent ink according to claim 2, is characterized in that, described graphene/carbon acid calcium/SiO
2compounded mix preparation method is as follows: be scattered in ethanol by graphene/carbon acid calcium compounded mix ultrasonic agitation; Add a certain proportion of water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and graphene/carbon acid calcium compounded mix after stirring is 1.8:1, adjust ph is 9, temperature of reaction is 25 DEG C, react 5 hours, carry out centrifugal and obtain precipitation 3 times by acetone and deionized water, washed with de-ionized water successively; This is deposited in 90
odry 2h under C, to obtain being coated with SiO
2graphene/carbon acid calcium/SiO
2compounded mix.
7. the preparation method of luminescent ink according to claim 6, it is characterized in that, the preparation method of described graphene/carbon acid calcium compounded mix is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 1000r/min centrifugal speed stir; 100g quantum dot calcium carbonate is added in 500ml deionized water, obtained calcium carbonate dispersion liquid after dispersion 240 ~ 300min under 1200 ~ 1500kW ultrasonic vibration and 1000 ~ 1200r/min centrifugal speed stir; In graphene dispersing solution, slowly drip calcium carbonate dispersion liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained graphene/carbon acid calcium compounded mix down 100kW is ultrasonic.
8. the preparation method of luminescent ink according to claim 2, is characterized in that, described Graphene/kaolin/SiO
2compounded mix preparation method is as follows: by Graphene/kaolin compounded mix ultrasonic agitation is scattered in ethanol; Add a certain proportion of water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and Graphene/kaolin compounded mix after stirring is 1.8:1, adjust ph is 9, temperature of reaction is 25 DEG C, react 5 hours, carry out centrifugal and obtain precipitation 3 times by acetone and deionized water, washed with de-ionized water successively; This is deposited in 90
odry 2h under C, to obtain being coated with SiO
2graphene/kaolin/SiO
2compounded mix.
9. the preparation method of luminescent ink according to claim 8, it is characterized in that, the preparation method of described Graphene/kaolin compounded mix is as follows: added by 1g Graphene in 100ml deionized water, obtained graphene dispersing solution after dispersion 180 ~ 200min under 800 ~ 1000kW ultrasonic vibration and 500 ~ 800r/min centrifugal speed stir; 50g nano kaoline is added in 500ml deionized water, obtained Dispersion of Kaolin liquid after dispersion 240 ~ 300min under 1000 ~ 1200kW ultrasonic vibration and 800 ~ 1000r/min centrifugal speed stir; In graphene dispersing solution, slowly drip Dispersion of Kaolin liquid, ultrasonic 30 ~ 60min, then suction filtration, oven dry, obtained Graphene/kaolin compounded mix down 100kW is ultrasonic.
10. the preparation method of luminescent ink according to claim 9, it is characterized in that, the preparation method of described nano-kaoline is as follows: by 150g kaolin ore with the rotating speed ball milling 60min of 1500 turns/min, then insert in 5L deionized water, add 220g Potassium ethanoate and stir 60min, suction filtration cleaning is about 7 to pH value, then with the rotating speed ball milling 60min of 1200 turns/min after drying under 80 degree of conditions, carry out 1800 turns/min ball milling under being adjusted to 300W ultrasonic wave again 1 hour, obtain the kaolin powder of particle diameter at 10 ~ 30nm.
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| CN105925063A (en) * | 2016-06-01 | 2016-09-07 | 佛山市高明区海帝陶瓷原料有限公司 | Fluorescent water-based ceramic three-dimensional printing ink and preparation method thereof |
| CN105949962A (en) * | 2016-07-18 | 2016-09-21 | 郑州四维特种材料有限责任公司 | Self-luminous epoxy resin liquid, preparation method of self-luminous epoxy resin liquid, self-luminous epoxy resin composite and self-luminous carbon fiber prepreg |
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| CN105949962B (en) * | 2016-07-18 | 2019-01-04 | 郑州四维特种材料有限责任公司 | A kind of self-luminous epoxy resin liquid and preparation method thereof, self-luminous epoxy resin composite material, self-luminous carbon fiber prepreg |
| CN106189507A (en) * | 2016-08-29 | 2016-12-07 | 佛山市高明区海帝陶瓷原料有限公司 | A kind of antibacterial noctilucence water-based ultraviolet (UV) curable ceramic ink jet ink and preparation method thereof |
| CN106366761A (en) * | 2016-08-29 | 2017-02-01 | 佛山市高明区海帝陶瓷原料有限公司 | Anti-bacterial luminous low-temperature ceramic ink for ink jet and preparation method thereof |
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