CN109401424A - A kind of cured high temperature sintering varnish of LED-UV cold light source and preparation method thereof - Google Patents
A kind of cured high temperature sintering varnish of LED-UV cold light source and preparation method thereof Download PDFInfo
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- CN109401424A CN109401424A CN201811098978.0A CN201811098978A CN109401424A CN 109401424 A CN109401424 A CN 109401424A CN 201811098978 A CN201811098978 A CN 201811098978A CN 109401424 A CN109401424 A CN 109401424A
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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
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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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
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
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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
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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Abstract
The present invention relates to cured high temperature sintering varnish of a kind of LED-UV cold light source and preparation method thereof, select compound resin, using reactive diluent and a variety of surfactants, add a variety of small-molecule substances, different resins are first separately handled, the technique that step-up temperature is uniformly mixed is carried out again, not only increase the flexibility that varnish prepares ink, glossiness, the adhesion for being needed on substrate is added after inorganic pigment prints in enhancing varnish, and improve the weatherability that varnish prepares ink, heat-proof aging, cold-resistant heat ageing, ultraviolet resistance aging, it is water-fast, acid-proof alkaline is splendid, the wearability that varnish prepares ink is improved simultaneously, extensibility and hardness.
Description
Technical field
The present invention relates to cured high temperature sintering varnish of a kind of LED-UV cold light source and preparation method thereof, belong to ink skill
Art field.
Background technique
Varnish, also known as cold stamp-pad ink, formulated oil, tempered oil, connection oil, blending cream etc., is mainly used for for adjusting oil
The adhesive and printing of ink.
High temperature varnish is that inorganic pigment is added to according to a certain percentage in high temperature varnish, by mixed grinding
It is configured to high temperature ink;Various colors ink will be prepared by way of printing is printed onto membranelle marble paper, also referred to as water transfer flower
On the paper special paper of water-soluble glue (a kind of precoat), then impregnated after wetting by water pattern is shifted be attached at object surface or
Printing is posted on ceramics or glass on heat transfer film by way of heat transfer.
However this high temperature varnish known in the art is the varnish of solvent volatile-type, uses thermoplasticity in formula
Acrylic resin, diluent use aromatic organic solvent, and solid content is lower, and ink performance is poor, while volatile organic solvent,
Slow drying speed low efficiency pollutes air and is harmful to the human body.
Summary of the invention
The object of the present invention is to provide cured high temperature sintering varnish of a kind of LED-UV cold light source and preparation method thereof, choosings
With compound resin, the reactive diluent of use and a variety of surfactants add a variety of small-molecule substances, and different resins are first divided
Processing is opened, then carries out the technique that step-up temperature is uniformly mixed, varnish is not only increased and prepares the flexibility of ink, gloss
Degree, enhancing varnish is needed on the adhesion of substrate after inorganic pigment printing is added, and improves varnish and prepare ink
Weatherability, heat-proof aging, cold-resistant heat ageing, ultraviolet resistance aging, water-fast, acid-proof alkaline is splendid, while improving varnish
Prepare the wearability, extensibility and hardness of ink.
A kind of cured high temperature sintering varnish of LED-UV cold light source, the formula including following parts by weight:
A kind of cured high temperature sintering varnish of LED-UV cold light source, preparation method are as follows:
S1, polyurethane acrylate resin, pure acrylate resins, reactive diluent are mixed, in 1200-1500r/min
Mixing speed under be dispersed with stirring 30-45min;
S2, addition light draw agent and continue to be dispersed with stirring, and temperature is controlled at 60-70 DEG C, is dispersed with stirring 30-45min;
S3, defoaming agent, levelling agent, thickening thixotropic agent are added after being completely dissolved disperse the present invention to can be obtained in 30-45 minutes
The cured high temperature sintering varnish of LED-UV cold light source.
Preferably, a kind of cured high temperature sintering varnish of LED-UV cold light source, further includes matching for following parts by weight
Side:
10-20 parts of terpene resin
10-15 parts of apple anhydride dehydration resin
Preferably, a kind of cured high temperature sintering varnish of LED-UV cold light source, further includes matching for following parts by weight
Side:
2-5 parts of surfactant
Preferably, a kind of cured high temperature sintering varnish of LED-UV cold light source, further includes matching for following parts by weight
Side:
Preferably, a kind of cured high temperature sintering varnish of LED-UV cold light source, preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 60-70%
The reactive diluent of dosage mixes, and is heated to 70-80 DEG C, is dispersed with stirring 30- under the mixing speed of 1200-1500r/min
60min is cooled to room temperature, spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 60-70 DEG C,
It is dispersed with stirring 30-60min under the mixing speed of 1200-1500r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, 35-45 DEG C is heated to, in the stirring of 500-700r/min
It is dispersed with stirring 60-80min under speed, adds surfactant and urea phosphate, is heated to 50-60 DEG C, in 800-1000r/min
Mixing speed under be dispersed with stirring 40-60min, continuously add photoinitiator and sodium lactate, be heated to 65-75 DEG C, in 1200-
It is dispersed with stirring under the mixing speed of 1500r/min to system and is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added, in 800-
40-80 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering tune of LED-UV cold light source of the present invention
Black oil.
Preferably, the invention also includes a kind of at least following technical characteristics:
The reactive diluent is by EM221 1,6- glycol diacrylate, EM222 dipropylene glycol diacrylate
Ester, EM223 tripropylene glycol diacrylate mix;
The photoinitiator is 2,2- dimethoxy -2- phenyl acetophenone (BDK), 1- hydroxy-cyciohexyl Benzophenone
(184), 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO), 2,4,6- trimethylbenzoyl-phenyl phosphine oxide
(TEPO) three kinds or more in;
The surfactant is Dodecyl Glucoside, in tea saponin, sodium lauryl sulfate, Tween-60, odium stearate
One or more.
The present invention also provides the varnish to prepare answering in water transfer or caloric transfer printing technology ink and its printing
With.
The present invention also provides a kind of cured high temperature sintering ink of LED-UV cold light source, the preparation method comprises the following steps: by of the invention
The ratio of varnish and the inorganic pigment 0.5-0.8:1 in mass ratio mixes, in the mixing speed of 1200-1500r/min
Under be dispersed with stirring to be uniformly mixed to get.
The present invention also provides the printing processes of the cured high temperature sintering ink of above-mentioned LED-UV cold light source:
1. using 200-420 mesh grid screen printing, it is printed on water-transfer printing paper or heat transfer film;
2. after being printed on water-transfer printing paper or heat transfer film, with LED-UV cold light source curing and drying 0.2-1s;
3. the water-transfer printing paper or heat transfer film after dry are transferred by water or caloric transfer printing technology is posted on material requested, lead to
500-1400 DEG C of high temperature sintering is crossed to form.
The present invention and the technology comparison of the varnish of solvent volatile-type in the prior art are as follows:
The invention has the benefit that
(1) present invention selects polyurethane acrylate resin, pure acrylate resins, terpene resin, apple anhydride dehydration tree
Rouge is as compound resin, not only solid content > 98%, but also improves flexibility, laser curing velocity, the glossiness of varnish, increases
The anti-knock properties and adhesion for being needed on substrate are added after inorganic pigment prints in strong varnish, and ink is made to be not easy to take off before sintering afterwards
It falls.
(2) reactive diluent that the present invention uses can decompose volatilization, to show the color of inorganic pigment in high temperature sintering
Phase controls the viscosity of varnish in 600-1200cps (mpas), thus good absorption inorganic pigment, while and
Other varnish compare, and organic solvent-free volatilization, volatile substance content is zero.
(3) present invention selects Dodecyl Glucoside, tea saponin, sodium lauryl sulfate, tween-in a variety of surfactants
60, one or more of odium stearate, the specific surfactant synergy of these types, improves above-mentioned compound resin
Emulsification system meets ink performance standard, can be improved the stability of compound resin, improves the weatherability of ink, corrosion-resistant
Property and wearability.
(4) present invention addition sodium carbonate, sodium sulfite, sodium pyrophosphate, urea phosphate, a variety of small-molecule substances such as sodium lactate with
Various kinds of resin polymer compounds the mechanical performance that can improve ink, and elasticity modulus, extensibility, hardness and other effects improve significant.
(5) the thickening thixotropic agent that the present invention adds can increase the thixotropic effects of varnish well, improve print when printing
Brush performance, while volatilization can be decomposed in the case of a high temperature.
(6) present invention uses and first separately handles different resins, then carries out the technique that step-up temperature is uniformly mixed, more
It is suitable for the characteristic of various different resins, is conducive to activate the functional group in each resin, can more protrude the advantageous of each resin
Effect.
Specific embodiment
Embodiment 1
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 60% dosage
Reactive diluent mixing, be heated to 70 DEG C, be dispersed with stirring 30min under the mixing speed of 1200r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 60 DEG C,
It is dispersed with stirring 30min under the mixing speed of 1200r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 35 DEG C, is stirred under the mixing speed of 500r/min
Dispersion 60min is mixed, surfactant and urea phosphate is added, is heated to 50 DEG C, the stirring point under the mixing speed of 800r/min
Dissipate 40min, continuously add photoinitiator and sodium lactate, be heated to 65 DEG C, be dispersed with stirring under the mixing speed of 1200r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added, 800/
40 minutes are dispersed with stirring under the mixing speed of min to get the cured high temperature sintering varnish of LED-UV cold light source of the present invention.
Wherein, polyurethane acrylate resin is aliphatic urethane diacrylate, is bought in Taiwan Changxing material supplier
Industry limited liability company, model 6141H-80.
Wherein, pure acrylate resins purchase is in Taiwan Changxing material industry limited liability company, model 6350-40.
Wherein, terpene resin purchase is in the prosperous forestry products Co., Ltd of Shanghai Songyuan.
Wherein, apple anhydride dehydration resin is 424# apple anhydride dehydration resin, is bought limited in the prosperous forestry products of Shanghai Songyuan
Company.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 100g, EM222 dipropylene glycol
Acid esters 100g, EM223 tripropylene glycol diacrylate 100g, mixes, and buys limited in Taiwan Changxing material industry share
Company.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 20g, 1- hydroxy-cyciohexyl Benzophenone
(184) mixture of 20g, 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO) 10g.
Wherein, defoaming agent is polymer-type defoaming agent, and model 085, levelling agent is acrylate leveling agent, model
348, purchase is in German Bi Ke BYK company.
Wherein, thickening thixotropic agent is that high-performance is micronized polyamide auxiliary rheological agents, and model SUPER, purchase is in France gram
Thunder Willie (CRA.UALLEY) company.
Wherein, surfactant is Dodecyl Glucoside 10g, tea saponin 5g, sodium lauryl sulfate 5g.
Embodiment 2
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 65% dosage
Reactive diluent mixing, be heated to 75 DEG C, be dispersed with stirring 40min under the mixing speed of 1400r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 65 DEG C,
It is dispersed with stirring 40min under the mixing speed of 1400r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 40 DEG C, is stirred under the mixing speed of 600r/min
Dispersion 70min is mixed, surfactant and urea phosphate is added, is heated to 55 DEG C, the stirring point under the mixing speed of 900r/min
Dissipate 50min, continuously add photoinitiator and sodium lactate, be heated to 70 DEG C, be dispersed with stirring under the mixing speed of 1400r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
60 minutes are dispersed with stirring under the mixing speed of 1000r/min to get the cured high temperature sintering inking of LED-UV cold light source of the present invention
Oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 200g, EM222 dipropylene glycol
Acid esters 200g, EM223 tripropylene glycol diacrylate 100g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 20g, 1- hydroxy-cyciohexyl Benzophenone
(184) 20g, 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO) 20g, 2,4,6- trimethylbenzoyl-phenyl
The mixture of phosphine oxide (TEPO) 20g.
Wherein, surfactant be Dodecyl Glucoside 5g, tea saponin 10g, sodium lauryl sulfate 5g, Tween-60 5g,
Odium stearate 5g.
Remaining is the same as embodiment 1.
Embodiment 3
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 70% dosage
Reactive diluent mixing, be heated to 80 DEG C, be dispersed with stirring 60min under the mixing speed of 1500r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 70 DEG C,
It is dispersed with stirring 60min under the mixing speed of 1500r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 45 DEG C, is stirred under the mixing speed of 700r/min
Dispersion 80min is mixed, surfactant and urea phosphate is added, is heated to 60 DEG C, the stirring point under the mixing speed of 1000r/min
Dissipate 60min, continuously add photoinitiator and sodium lactate, be heated to 75 DEG C, be dispersed with stirring under the mixing speed of 1500r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
80 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering inking of LED-UV cold light source of the present invention
Oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 200g, EM222 dipropylene glycol
Acid esters 200g, EM223 tripropylene glycol diacrylate 400g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 30g, 1- hydroxy-cyciohexyl Benzophenone
(184) 30g, 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO) 20g, 2,4,6- trimethylbenzoyl-phenyl
The mixture of phosphine oxide (TEPO) 20g.
Wherein, surfactant is Dodecyl Glucoside 15g, tea saponin 15g, sodium lauryl sulfate 10g, odium stearate
10g。
Remaining is the same as embodiment 1.
Embodiment 4
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 60% dosage
Reactive diluent mixing, be heated to 70 DEG C, be dispersed with stirring 40min under the mixing speed of 1300r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 60 DEG C,
It is dispersed with stirring 40min under the mixing speed of 1300r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 35 DEG C, is stirred under the mixing speed of 500r/min
Dispersion 60min is mixed, surfactant and urea phosphate is added, is heated to 50 DEG C, the stirring point under the mixing speed of 800r/min
Dissipate 45min, continuously add photoinitiator and sodium lactate, be heated to 65 DEG C, be dispersed with stirring under the mixing speed of 1300r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
50 minutes are dispersed with stirring under the mixing speed of 900r/min to get the cured high temperature sintering inking of LED-UV cold light source of the present invention
Oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 100g, EM222 dipropylene glycol
Acid esters 200g, EM223 tripropylene glycol diacrylate 100g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 20g, 2,4,6- trimethylbenzoyls
The mixture of base-diphenyl phosphine oxide (TPO) 20g, 2,4,6- trimethylbenzoyl-phenyl phosphine oxide (TEPO) 20g.
Wherein, surfactant is Dodecyl Glucoside 5g, tea saponin 10g, Tween-60 5g, odium stearate 5g.
Remaining is the same as embodiment 1.
Embodiment 5
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 70% dosage
Reactive diluent mixing, be heated to 80 DEG C, be dispersed with stirring 50min under the mixing speed of 1400r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 70 DEG C,
It is dispersed with stirring 55min under the mixing speed of 1400r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 45 DEG C, is stirred under the mixing speed of 700r/min
Dispersion 75min is mixed, surfactant and urea phosphate is added, is heated to 60 DEG C, the stirring point under the mixing speed of 1000r/min
Dissipate 55min, continuously add photoinitiator and sodium lactate, be heated to 75 DEG C, be dispersed with stirring under the mixing speed of 1400r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
70 minutes are dispersed with stirring under the mixing speed of 1100r/min to get the cured high temperature sintering inking of LED-UV cold light source of the present invention
Oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 200g, EM222 dipropylene glycol
Acid esters 300g, EM223 tripropylene glycol diacrylate 200g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 40g, 1- hydroxy-cyciohexyl Benzophenone
(184) 30g, 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO) 10g, 2,4,6- trimethylbenzoyl-phenyl
The mixture of phosphine oxide (TEPO) 10g.
Wherein, surfactant is Dodecyl Glucoside 10g, tea saponin 10g, sodium lauryl sulfate 5g, Tween-60
10g, odium stearate 5g.
Remaining is the same as embodiment 1.
Embodiment 6
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 60% dosage
Reactive diluent mixing, be heated to 80 DEG C, be dispersed with stirring 60min under the mixing speed of 1200r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 60 DEG C,
It is dispersed with stirring 30min under the mixing speed of 1500r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 45 DEG C, is stirred under the mixing speed of 500r/min
Dispersion 80min is mixed, surfactant and urea phosphate is added, is heated to 50 DEG C, the stirring point under the mixing speed of 1000r/min
Dissipate 40min, continuously add photoinitiator and sodium lactate, be heated to 75 DEG C, be dispersed with stirring under the mixing speed of 1200r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
40-80 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering tune of LED-UV cold light source of the present invention
Black oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 500g, EM222 dipropylene glycol
Acid esters 200g, EM223 tripropylene glycol diacrylate 100g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 10g, 1- hydroxy-cyciohexyl Benzophenone
(184) mixture of 20g, 2,4,6- trimethylbenzoyl-phenyl phosphine oxide (TEPO) 20g.
Wherein, surfactant is tea saponin 5g, sodium lauryl sulfate 5g, Tween-60 5g, odium stearate 5g.
Remaining is the same as embodiment 1.
Embodiment 7
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
Preparation method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 70% dosage
Reactive diluent mixing, be heated to 75 DEG C, be dispersed with stirring 60min under the mixing speed of 1200r/min, be cooled to room temperature,
It is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 65 DEG C,
It is dispersed with stirring 60min under the mixing speed of 1200r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, is heated to 40 DEG C, is stirred under the mixing speed of 500r/min
Dispersion 80min is mixed, surfactant and urea phosphate is added, is heated to 55 DEG C, the stirring point under the mixing speed of 800r/min
Dissipate 60min, continuously add photoinitiator and sodium lactate, be heated to 70 DEG C, be dispersed with stirring under the mixing speed of 1200r/min to
System is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
60 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering inking of LED-UV cold light source of the present invention
Oil.
Wherein, reactive diluent is by EM221 1, two propylene of 6- glycol diacrylate 200g, EM222 dipropylene glycol
Acid esters 50g, EM223 tripropylene glycol diacrylate 50g is mixed.
Wherein, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone (BDK) 25g, 1- hydroxy-cyciohexyl Benzophenone
(184) 25g, 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO) 25g, 2,4,6- trimethylbenzoyl-phenyl
The mixture of phosphine oxide (TEPO) 25g.
Wherein, surfactant is Dodecyl Glucoside 10g, tea saponin 15g, sodium lauryl sulfate 10g, Tween-60
10g, odium stearate 5g.
Remaining is the same as embodiment 1.
Comparative example 1
The difference from embodiment 1 is that:
By the terpene resin in Malin's acid resin (purchase is in the prosperous forestry products Co., Ltd of Shanghai Songyuan) alternative embodiment 1.
Comparative example 2
The difference from example 2 is that:
By the mistake in #210 rosin modified phenolic resin (purchase is in the prosperous forestry products Co., Ltd of Shanghai Songyuan) alternative embodiment 2
Water apple anhydride resin.
Comparative example 3
Difference with embodiment 3 is:
By the tea saponin in hydroxyethyl cellulose alternative embodiment 3.
Comparative example 4
Difference with embodiment 4 is:
By the sodium carbonate in sodium bicarbonate alternative embodiment 4.
Comparative example 5
Difference with embodiment 5 is:
By the sodium lactate in sodium iso-octoate alternative embodiment 5.
Comparative example 6
Difference with embodiment 6 is:
Preparation method are as follows:
S1, polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, activity are diluted
Agent, terpene resin, sodium sulfite, sodium pyrophosphate mixing, are heated to 80 DEG C, are dispersed with stirring under the mixing speed of 1200r/min
60min is cooled to room temperature, spare;
S2, surfactant, urea phosphate, photoinitiator and sodium lactate is added in the intermediate of step S1, is heated to 75 DEG C,
It is dispersed with stirring under the mixing speed of 1200r/min to system and is uniformly mixed;
S3, the homogenous intermediate of step S2 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added,
40-80 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering tune of LED-UV cold light source of the present invention
Black oil.
Comparative example 7
Difference with embodiment 7 is:
A kind of cured high temperature sintering varnish of LED-UV cold light source, is made of formula as below:
The invention is not limited to above-mentioned specific embodiment, those skilled in the art can also make a variety of variations accordingly,
But it is any all to cover within the scope of the claims with equivalent or similar variation of the invention.
Test example 1:
By varnish made from each embodiment and comparative example and inorganic pigment (ferric oxide red colorant) in mass ratio 0.6:
1 ratio mixing, is dispersed with stirring to uniformly mixed to get each embodiment and comparative example under the mixing speed of 1500r/min
Ink obtained carries out following tests, printing technology are as follows:
1. using 300 mesh grid screen printings, ink is printed on water-transfer printing paper;
2. after being printed on water-transfer printing paper, with LED-UV cold light source curing and drying 0.5s;
3. the ink after dry on water-transfer printing paper is posted on material requested by water transfer printing technique, pass through 800 DEG C of height
Temperature is sintered.
(1) adhesive force is tested
Adhesive force test is carried out to sample, using hundred lattice methods of testing, ink is made in each embodiment and comparative example and passes through
The identical straight line scratch in lower 10 intervals is drawn every 1-1.2mm on the workpiece that above-mentioned water transfer printing technique is posted, in straight line scratch
Upright position draw 10 identical scratches in interval again, become the square of 100 lattice for 10 × 10, knife is drawn and be cut when going down
To seeing ground, it is not possible to only cut on ink, otherwise test just invalid.It, can or can not with adhesive tape test after knife has been drawn
Fall off (adhesive tape is 3m600 adhesive tape), firstly, adhesive tape is affixed on the position for pulling hundred lattice, is depressed with finger and tightly attaches adhesive tape, then
Adhesive tape is opened with the power of moment, whether the ink seen on workpiece has obscission.The results are shown in Table 2.
100 lattice test evaluation standard of table
Iso grade is international standard grade, and Astm grade is Unite States Standard grade.
(2) flexibility is tested
Ink is made in each embodiment and comparative example to be posted on tinplate by above-mentioned water transfer printing technique, then according to
Standard GB/T/T1731-93 " paint film flexibility measuring method " measures the flexibility of ink.The results are shown in Table 2.
(3) glossiness is tested
Ink is made in each embodiment and comparative example to be printed on blank sheet of paper with screen process press, by national standard GB9754-88
It is required to be tested, the instrument connection of glossiness tester is directed at the place printed, reads its gloss after number is stablized
Degree.The results are shown in Table 2.
The prior art in this test example uses Chinese patent ZL201610544262.3, and entitled " a kind of LED is cured
Water transfer ink and preparation method thereof " in embodiment 1 preparation method.
The varnish that 2 present invention of table obtains prepares the adhesive force after ink, flexibility, glossiness effect
It can be seen that the varnish that the embodiment of the present invention 1-7 is obtained from upper watch test result and prepare ink again, carry out attached
Put forth effort, after the test of flexibility, glossiness, adhesive force is stronger, and flexibility is preferable, can achieve optimal level, and glossiness is more excellent, can
To reach 102 or more, said effect is substantially better than comparative example 1 (replacing a kind of resin), comparative example 2 (replacing another resin),
Relatively better than comparative example 3 (replacement surfactant), comparative example 6 (preparation process is different), comparative example 7 (raw material proportioning is different) and existing
There is technical patent, is not much different with comparative example 4 (replacing a kind of small molecule 1), comparative example 5 (replacing another small molecule).It can be seen that
Polyurethane acrylate resin that the present invention uses, pure acrylate resins, terpene resin, apple anhydride dehydration resin are as compound
Compared with other resins ink flexibility, glossiness can be improved, after inorganic pigment printing is added in enhancing varnish in resin
Adhesion;One of dialkyl group glucosides, tea saponin, sodium lauryl sulfate, Tween-60, odium stearate or several are selected simultaneously
Kind is used as specific surfactant, improves the emulsification system of above-mentioned compound resin, right compared with other surfactants
The flexibility of ink, glossiness, adhesive force slightly improve;The difference of sequence and temperature in preparation process, also can be to ink
Flexibility, glossiness, adhesive force have an impact.Therefore, the present invention uses polyurethane acrylate resin, pure acrylate resins, terpene
Olefine resin, apple anhydride dehydration resin select specific surfactant as compound resin, first separate using by different resins
Processing, then the technique that step-up temperature is uniformly mixed is carried out, it improves varnish and prepares the flexibility of ink, glossiness, increase
The adhesion for being needed on substrate is added after inorganic pigment prints in strong varnish, keeps ink rear not easily to fall off before sintering.
Test example 2
By varnish made from each embodiment and comparative example and inorganic pigment (lead chromate yellow pigment) 0.5:1 in mass ratio
Ratio mixing, be dispersed with stirring under the mixing speed of 1500r/min to be uniformly mixed to get each embodiment and comparative example system
The ink obtained carries out following tests, printing technology are as follows:
1. using 300 mesh grid screen printings, ink is printed on water-transfer printing paper;
2. after being printed on water-transfer printing paper, with LED-UV cold light source curing and drying 0.5s;
3. the ink after dry on water-transfer printing paper is posted on sample (glass of 20cm × 20cm) by water transfer printing technique,
It is formed by 800 DEG C of high temperature sintering.
(1) weatherability is tested
1. heat ageing: sample being put into 57 DEG C of baking oven and toasted, taken out after 48 hours and see whether to burst, such as not
Explosion, then above-mentioned adhesive force test is carried out, with Iso descriptive grade.
2. cold and hot aging: sample place hot-cool environment in, with -18 DEG C environment 4 hours, room temperature 2 hours, 57 DEG C of environment 4
Hour, room temperature 2 hours, for a circulation, taking-up saw whether to burst after carrying out 2 circulations, did not burst such as, then carry out
Adhesive force test is stated, with Iso descriptive grade.
3. ultraviolet light and aging: sample being put into and is filled by the accelerated test that xenon provides high-intensity ultraviolet light as ultraviolet lamp source
It sets, is exposed to the sun test by 18 hours high intensity, taking-up sees whether to burst, and does not burst such as, then carry out above-mentioned adhesive force
Test, with Iso descriptive grade.
4. water resistance: sample all being impregnated in deionized water, is taken out after 24 hours and sees whether to burst, such as not
Explosion, then above-mentioned adhesive force test is carried out, with Iso descriptive grade.
5. resistance to acid and alkali: sample being all immersed in the hydrochloric acid solution of 0.2mol/L, take out and see whether after 10 hours
It bursts, does not burst such as, then carry out above-mentioned adhesive force test, with Iso descriptive grade.
Sample is all immersed in the sodium hydroxide solution of 0.2mol/L, taking-up sees whether to occur quick-fried after 10 hours
It splits, does not burst such as, then carry out above-mentioned adhesive force test, with Iso descriptive grade.
The above test result is as shown in table 3;
The prior art in this test example uses Chinese patent ZL201610544262.3, and entitled " a kind of LED is cured
Water transfer ink and preparation method thereof " in embodiment 1 preparation method.
The varnish that 3 present invention of table obtains prepares the weatherability effect (whether bursting, Iso grade) after ink
It can be seen that the varnish that the embodiment of the present invention 1-7 is obtained from upper watch test result and prepare ink again, carry out resistance to
After the test of time property, heat-proof aging, cold-resistant heat ageing, ultraviolet resistance aging, water-fast, acid and alkali-resistance, said effect are substantially better than ratio 3
(replacement surfactant), relatively better than comparative example 4 (replacing a kind of small molecule), comparative example 5 (replacing another small molecule) comparison
Example 6 (preparation process is different), comparative example 7 (raw material proportioning is different) and prior art patent, (replace a kind of tree with comparative example 1
Rouge), comparative example 2 (replace another resin) is not much different.It can be seen that the present invention selects dodecyl in a variety of surfactants
One or more of glucosides, tea saponin, sodium lauryl sulfate, Tween-60, odium stearate, the specific surface-active of these types
Agent synergy is compared with others surfactant, can be improved the stability of compound resin, improve the weather-proof of ink
Property, corrosion resistance;Add sodium carbonate, sodium sulfite, sodium pyrophosphate, urea phosphate, a variety of small-molecule substances such as sodium lactate with it is a variety of
Resinous polymer compounding, and other small molecular phases compare, and can improve the mechanical performance of ink, and enhancing ink is weather-proof slightly
Property;The difference of sequence and temperature in preparation process can also have an impact to the weatherability of ink.Therefore, the present invention is using selection
One or more of Dodecyl Glucoside, tea saponin, sodium lauryl sulfate, Tween-60, odium stearate, these types are specific
Surfactant synergy, improves the emulsification system of above-mentioned compound resin, addition sodium carbonate, sodium sulfite, sodium pyrophosphate,
A variety of small-molecule substances such as urea phosphate, sodium lactate are compounded with various kinds of resin polymer, are first separately handled using by different resins, then
The technique that step-up temperature is uniformly mixed is carried out, improves the weatherability that varnish prepares ink, heat-proof aging, cold-hot are old
Change, ultraviolet resistance aging, water-fast, acid-proof alkaline is splendid.
Test example 3:
By varnish made from each embodiment and comparative example and inorganic pigment (chrome oxide green pigment) in mass ratio 0.8:
1 ratio mixing, is dispersed with stirring to uniformly mixed to get each embodiment and comparative example under the mixing speed of 1500r/min
Ink obtained carries out following tests, printing technology are as follows:
1. using 300 mesh grid screen printings, ink is printed on water-transfer printing paper;
2. after being printed on water-transfer printing paper, with LED-UV cold light source curing and drying 0.5s;
3. the ink after dry on water-transfer printing paper is posted on sample by water transfer printing technique, burnt by 1000 DEG C of high temperature
It ties.
(1) wearability test
Ink coating wearability: multifunctional alcohol rubber friction testing machine (model: LX-5600, the prosperous instrument of Dongguan benefit is used
Instrument factory) test, load 500g, the results are shown in Table 4.
The representation method of wearability: 1 grade to be worst, 5 grades are optimal.
(2) extensibility is tested
Using thin-film material tensile strength testing system, the ink on water-transfer printing paper after drying is made into the standard of dumbbell shape
Sample carries out extension test to tensilometer, is averaged after doing 3 tests, the results are shown in Table 4.
(3) hardness test
Ink layer of ink hardness: measuring pencil durometer, GB/T 6739-2006, the results are shown in Table 4.
(4) volatile substance content measuring
The method of mock standard CY/T 132.1-2015,80 DEG C of Static Headspace sample introductions carry out volatility to ink obtained
Organic compound monitoring, the results are shown in Table 4, and the TOVC of detection here is mainly toluene.
The prior art in this test example is existing solvent volatility varnish.
The varnish that 4 present invention of table obtains prepares the wearability after ink, extensibility, hardness, volatile substance content effect
It can be seen that the varnish that the embodiment of the present invention 1-7 is obtained from upper watch test result and prepare ink again, carry out resistance to
After mill property, extensibility, hardness, volatile substance content measuring, abrasion resistance and hardness is stronger, can achieve optimal level, extensibility
Longer, volatile substance content is without said effect is substantially better than comparative example 4 (replacing a kind of small-molecule substance), (replacement of comparative example 5
Another small-molecule substance), relatively better than comparative example 3 (replacement surfactant), ratio 6 (preparation process is different), comparative example 7
(raw material proportioning is different) and the prior art are differed with comparative example 1 (replacing a kind of resin), comparative example 2 (replacing another resin)
Less.It can be seen that present invention addition sodium carbonate, sodium sulfite, sodium pyrophosphate, urea phosphate, a variety of small-molecule substances such as sodium lactate and more
Kind resinous polymer compounding, compared with other small-molecule substances, so that the wearability of ink, extensibility, hardness and other effects mention
One or more of it is high significant, while selecting dialkyl group glucosides, tea saponin, sodium lauryl sulfate, Tween-60, odium stearate
As specific surfactant, the emulsification system and other surfaces activating agent for improving above-mentioned compound resin compare, to ink
Wearability, extensibility, hardness improves;The difference of sequence and temperature in preparation process, also can be to the resistance to of ink
Mill property, extensibility, hardness have an impact.Therefore, the present invention adds sodium carbonate, sodium sulfite, sodium pyrophosphate, urea phosphate, sodium lactate
The mechanical performance that can improve ink is compounded with various kinds of resin polymer etc. a variety of small-molecule substances, using selection dodecyl sugar
One or more of glycosides, tea saponin, sodium lauryl sulfate, Tween-60, odium stearate, the specific surfactant of these types
Synergy improves the emulsification system of above-mentioned compound resin, and different resins is first separately handled, then carries out step-up temperature and stir
Uniformly mixed technique is mixed, wearability, extensibility and hardness that varnish prepares ink are improved.
Claims (10)
1. a kind of cured high temperature sintering varnish of LED-UV cold light source, it is characterized in that: the formula including following parts by weight:
2. a kind of cured high temperature sintering varnish of LED-UV cold light source as described in claim 1, it is characterized in that: its preparation side
Method are as follows:
S1, polyurethane acrylate resin, pure acrylate resins, reactive diluent are mixed, in stirring for 1200-1500r/min
It mixes and is dispersed with stirring 30-45min under speed;
S2, addition photoinitiator continue to be dispersed with stirring, and temperature is controlled at 60-70 DEG C, is dispersed with stirring 30-45min;
S3, defoaming agent, levelling agent, thickening thixotropic agent are added after being completely dissolved, being dispersed with stirring 30-45 minutes can be obtained the present invention
The cured high temperature sintering varnish of LED-UV cold light source.
3. a kind of cured high temperature sintering varnish of LED-UV cold light source as described in claim 1, it is characterized in that: further include with
The formula of lower parts by weight:
10-20 parts of terpene resin
10-15 parts of apple anhydride dehydration resin.
4. a kind of cured high temperature sintering varnish of LED-UV cold light source as claimed in claim 3, it is characterized in that: further include with
The formula of lower parts by weight:
2-5 parts of surfactant.
5. a kind of cured high temperature sintering varnish of LED-UV cold light source as claimed in claim 4, it is characterized in that: further include with
The formula of lower parts by weight:
6. a kind of cured high temperature sintering varnish of LED-UV cold light source as claimed in claim 5, it is characterized in that: its preparation side
Method are as follows:
S1, by polyurethane acrylate resin, pure acrylate resins, apple anhydride dehydration resin, sodium carbonate, 60-70% dosage
Reactive diluent mixing, be heated to 70-80 DEG C, be dispersed with stirring 30-60min under the mixing speed of 1200-1500r/min,
It is cooled to room temperature, it is spare;
S2, by terpene resin, sodium sulfite, sodium pyrophosphate, remaining reactive diluent mixing is heated to 60-70 DEG C,
It is dispersed with stirring 30-60min under the mixing speed of 1200-1500r/min, is cooled to room temperature, it is spare;
S3, the obtained intermediate of step S1 and S2 are mixed, 35-45 DEG C is heated to, in the mixing speed of 500-700r/min
Under be dispersed with stirring 60-80min, add surfactant and urea phosphate, be heated to 50-60 DEG C, in stirring for 800-1000r/min
It mixes and is dispersed with stirring 40-60min under speed, continuously add photoinitiator and sodium lactate, be heated to 65-75 DEG C, in 1200-1500r/
It is dispersed with stirring under the mixing speed of min to system and is uniformly mixed;
S4, the homogenous intermediate of step S3 is cooled to room temperature, defoaming agent, levelling agent, thickening thixotropic agent is added, in 800-
40-80 minutes are dispersed with stirring under the mixing speed of 1200r/min to get the cured high temperature sintering tune of LED-UV cold light source of the present invention
Black oil.
7. the cured high temperature sintering varnish of a kind of LED-UV cold light source as described in claim 1 or 4 or 6, it is characterized in that: also
Including a kind of at least following technical characteristic:
The reactive diluent is by 1,6- glycol diacrylate, dipropylene glycol diacrylate, tripropylene glycol dipropyl
Olefin(e) acid ester mixes;
The photoinitiator is 2,2- dimethoxy -2- phenyl acetophenone, 1- hydroxy-cyciohexyl Benzophenone, 2,4,6- front three
Three kinds or more in base benzoyl-diphenyl phosphine oxide, 2,4,6- trimethylbenzoyl-phenyl phosphine oxide;
The surfactant is Dodecyl Glucoside, tea saponin, sodium lauryl sulfate, Tween-60, one in odium stearate
Kind is several.
8. varnish as claimed in claim 6 is preparing the application in water transfer or caloric transfer printing technology ink and its printing.
9. application as claimed in claim 8, it is characterized in that: ink the preparation method comprises the following steps: the varnish and inorganic pigment
The ratio of 0.5-0.8:1 in mass ratio mixes, and is dispersed with stirring under the mixing speed of 1200-1500r/min to being uniformly mixed, i.e.,
?.
10. application as claimed in claim 8 or 9, it is characterized in that: the printing process of ink are as follows:
1. using 200-420 mesh grid screen printing, it is printed on water-transfer printing paper or heat transfer film;
2. after being printed on water-transfer printing paper or heat transfer film, with LED-UV cold light source curing and drying 0.2-1s;
3. the water-transfer printing paper or heat transfer film after dry are transferred by water or caloric transfer printing technology is posted on material requested, pass through
500-1400 DEG C of high temperature sintering forms.
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Application publication date: 20190301 |