CN103436094A - Thermosetting high temperature resisting printing ink for touch screen as well as preparation method of printing ink - Google Patents
Thermosetting high temperature resisting printing ink for touch screen as well as preparation method of printing ink Download PDFInfo
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Abstract
The invention discloses thermosetting high temperature resisting printing ink for a touch screen as well as a preparation method of the printing ink. The formula of the printing ink comprises the following raw materials in parts by weight: 55-65 parts of modified organic silicon resin, 20-30 parts of titanium dioxide, 5-15 parts of powder packing, 3-8 parts of a diluent, 0.5-1.4 parts of a dispersant, 0.1-0.3 part of a leveling agent, 0.05-0.1 part of a defoamer, 1-2 parts of a silane coupling agent and 2-5 parts of a curing agent. The preparation method comprises the following steps: mixing the modified organic silicon resin, a pigment, the powder packing, 0.35-0.95 part of the dispersant, 0.05-0.15 part of the leveling agent and 2-5.4 parts of the diluent to obtain a main agent; and adding the curing agent, the defoamer, the silane coupling agent as well as remaining leveling agent, dispersant and diluent into the main agent, and dispersing, filtering and discharging. The printing ink coating is high temperature- resisting in coating, excellent in color retention at a high temperature of 300 DEG C, good in adhesion to a base material, high in hardness, resistant to acetone wiping and resistant to ITO (Indium Tin Oxides) etching liquids.
Description
Technical field
The present invention relates to technical field of ink, particularly relate to high temperature resistant touch screen printing ink of a kind of thermoset and preparation method thereof.
Background technology
At present touch screen is used widely in fields such as smart mobile phone, panel computer, super utmost point basis, touch screen 3D TVs, along with the raising of people's quality of life, and also can be more and more higher to the performance requriements of touch screen; In future, the touch screen of production large size, high precision, super sensitivity will be to be engaged in the core competitiveness place that produces touch screen enterprise; Touch screen printing ink is not only protection and the effect of decorating to touch screen, more directly affects the quality of ITO plated film, and to touch screen, sensitivity has material impact;
General mechanical properties such as gathering (ammonia) ester, epoxy resin and the good resin system of endurance of using of current commercially available touch screen printing ink done ink adhesive, but the easy xanthochromia of coating or cracking after carrying out 280 ℃ of high temperature ITO coating process, thereby the use of high temperature ITO coating process of restriction, and then limited the further raising of touch screen sensitivity;
The silicone resin of epoxy resin and polyester modification, can combine mechanical property and the endurance of the thermotolerance of silicone resin excellence and water tolerance and epoxy resin, polyester excellence; Zhang Jianhuas etc. adopted in unsaturated polyester post-synthesis phase, added the organosilicon performed polymer, utilized condensation reaction to prepare organosilicon modified polyester, and it is thermally-stabilised good, 320 ℃ of heat decomposition temperatures, and good mechanical properties is widely applied aspect solvent-free immersion paint; Tao Zhi waits by force and adopts epoxy resin modified organosilicon, and the resin thermal weight loss test (TGA) of preparation shows, completely crued modified resin before 300 ℃ without any weight loss, and good mechanical properties, water tolerance is also better; As ink adhesive, can prepare high temperature resistant tint retention and good mechanical properties, endurance touch screen printing ink preferably with this type of modified organic silicone resin;
Summary of the invention
The object of the present invention is to provide a kind of anti-300 ℃ to have stable high-temperature performance, tint retention is good, the mechanical property excellence, and anti-acetone 50 nothings of wiping repeatedly comes off, without the high temperature resistant touch screen printing ink of thermoset faded.
Another purpose of the present invention is in the preparation method that the high temperature resistant touch screen printing ink of a kind of described thermoset is provided.
Purpose of the present invention realizes by following technical solution:
A kind of thermoset is high temperature resistant touch screen printing ink, in parts by weight, the raw material of its formula consists of:
Described modified organic silicone resin is one or both in polyester modified organic silicon resin and epoxy modified silicone resin;
Described pigment powder is Rutile type Titanium Dioxide and charcoal blacks;
Described dispersion agent is modified polyurethane superpolymer, polyester modification poly phosphate and containing one or more in the interpolymer solution of acidic-group;
Described powder filler is one or more in nano silicon, glass powder, mica powder and talcum powder;
Described thinner is the DBE(dicarboxylic acid esters), one or more in isophorone, 200 solvent oils, pimelinketone and dimethylbenzene;
Described flow agent is one or more in type siloxane flow agent and non-silicon class flow agent; Described type siloxane flow agent is Silok8144 or Silok8244; Described non-silicon class flow agent is AFCONA3777s or AFCONA3670;
Described defoamer is one or more in modified polyorganosiloxane and non-silicon defoamer; Described modified polyorganosiloxane is AFCONA2022, GSK-716 or SD-100; Described non-silicon defoamer is AFCONA2720;
Described silane coupling agent is one or more in propyl trimethoxy silicane A187, propyl trimethoxy silicane Z6121 and propyl-triethoxysilicane KH550; The described interpolymer solution containing acidic-group is one or more in TEGO628, BYK110 and Silok7160;
Described solidifying agent is one or more in methyl-etherified terpolycyantoamino-formaldehyde resin CYMEL 303 solidifying agent, amino terpolycyantoamino-formaldehyde resin CYMEL 325 solidifying agent and isocyanic ester BL 3175, IPDI solidifying agent;
During preparation, in formulation weight part, get modified organic silicone resin, pigment, powder filler, 0.35-0.95 part dispersion agent, 0.05-0.15 part flow agent and 2-5.4 part mixing diluents, grinding distribution, prepare host; By solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, add in described host after 1-2.6 part mixing diluents stirs, the rear filtration that is uniformly dispersed, and discharging obtains the high temperature resistant touch screen printing ink of thermoset; Described dispersion agent, flow agent and twice consumption sum of thinner are parts by weight in formula material.
For further realizing the object of the invention, preferably, described titanium dioxide is Tupont902
+, one or more in Tiona595 and TionaRCL69.Described carbon black is one or more in T1, N330 and TH311.Described modified polyurethane superpolymer is AFCONA4010 or AFCONA4071; Described polyester modification poly phosphate is AFCONA5010 or AFCONA5210.Described polyester modified organic silicon resin is JY7200, YS-133 or KE-561.Described epoxy modified silicone resin is SH-023-4, HR-10 or HG-52.
The preparation method of described thermoset is high temperature resistant touch screen printing ink comprises the steps and processing condition:
1) in the composition of raw materials weight part, get modified organic silicone resin, add pigment, powder filler, 0.35-0.95 part dispersion agent, 0.05-0.15 part flow agent, 2-5.4 part thinner, at 2000-2500rpm grinding distribution 1h-1.5h, obtain host;
2) in the composition of raw materials weight part, get solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, 1-2.6 part thinner is in beaker, after stirring, join in described host, under dispersing speed 1000-1500rpm, disperse to filter after 0.5h-1h, discharging obtains the high temperature resistant touch screen printing ink of thermoset;
Described dispersion agent, flow agent and twice consumption sum of thinner are parts by weight in formula material.
During touch screen printing ink use that this thermoset is high temperature resistant, comprise the steps:
1), by the high temperature resistant touch screen printing ink prepared, add 2-15 part mixed diluting dilution agent by its weight part, mixed diluent is by dimethylbenzene, pimelinketone, isophorone, DBE(dibasic ester) in two or more form.Adjusting viscosity to construction is applicable to viscosity number;
2) with the ZBQ-4 coating device, at base material (glass, tinplate etc.), film, after 180 ℃ of-200 ℃ of 1h of baking oven baking or 250 ℃ of 25min solidify high temperature resistant printing ink coating;
With respect to prior art, the present invention has following advantage:
1) the high temperature resistant touch screen printing ink provided, adopt the silicone resin of modification as binder, has good resistance toheat, and high temperature resistant 300 ℃/100min films complete, and tint retention is good, flawless.
2) hydroxyl on modified organic silicone resin under certain condition, can with solidifying agent in the active group cross-linking and curing reaction, make paint film there is tridimensional network, make its glass surface have good sticking power, simultaneously high, the water-tolerant of hardness of film, anti-acetone wiping and ITO etching solution to soak paint film complete;
Embodiment
Below in conjunction with embodiment, the present invention is explained in detail, purpose is better to understand the content of the present patent application for the public, rather than to the restriction of the described technology contents of the present patent application.Any increase and decrease of doing in not violating the present patent application invention spirit, replacement, improvement are all within the present patent application technical scheme required for protection.
Embodiment 1
1) get 55 polyester modified organic silicon resin JY7200(Dongguan Jun Yi Chemical Industry Science Co., Ltd), 20g Tupont902
+titanium dioxide (E.I.Du Pont Company), 3g glass powder, the 2g nano silicon, 1g isophorone, 1g200 solvent oil, 0.3g BYK110 dispersion agent (BYK auxiliary agent), 0.1g AFCONA3670 flow agent (dust husband Kona chemistry), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) get 1g CYMEL303,1g CYMEL325 linking agent (Weng Kaier company limited), the 2g pimelinketone, 0.5g KH550 coupling agent, 0.5g A187 coupling agent, 0.2g AFCONA-5010 dispersion agent (dust husband Kona chemistry), 0.1g AFCONA3777s flow agent (dust husband Kona chemistry) adds in described host, filters discharging after dispersion 30min and obtain ink product under the 1000rpm rotating speed;
3) by the high temperature resistant touch screen printing ink prepared, add high temperature resistant touch screen ink by weight 8% mixed diluent (mixed diluent by isophorone and pimelinketone in mass ratio 1:1 be mixed to get) dilution, adjusting viscosity is to the working viscosity value, film with the ZBQ-4 coating device, after 180 ℃ of 1h of baking oven baking solidify, obtain high temperature resistant printing ink coating; The Performance Detection situation of printing ink coating that gained is high temperature resistant is as shown in table 1.
Embodiment 2
1) get 60g epoxy modified silicone resin HG-52(Zhong Hao Chenguang Research Institute of Chemical Industry company limited), 10g Tiona-RCL69 titanium dioxide (the grand industry of Shanghai well), 15g Tiona-595 titanium dioxide (the grand industry of Shanghai well), 5g glass powder, the 2g nano silicon, the 1g talcum powder, the 1g isophorone, 0.3g AFCONA5010 dispersion agent (dust husband Kona chemistry), 0.3g AFCONA4010 dispersion agent (dust husband Kona chemistry), 0.1g AFCONA3777s flow agent (dust husband Kona chemistry), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host,
2) get 2.25g CYMEL325 linking agent (Weng Kaier company limited), 2g DBE(dicarboxylic acid esters), 1g A-187 coupling agent, 1g KH550 coupling agent, 0.3g TEGO-628 dispersion agent (the high auxiliary agent of enlightening), 0.1g AFCONA3670 flow agent (dust husband Kona chemistry), 0.05g GSK-716 defoamer (Gauss advances fine chemistry industry), join in host, filter discharging after dispersion 30min under the 1200rpm rotating speed and obtain ink product;
3) by the high temperature resistant touch screen printing ink prepared, add high temperature resistant touch screen ink by weight 10% mixed diluent (mixed diluent by dicarboxylic acid esters and pimelinketone in mass ratio 1:1 be mixed to get) dilution, adjusting viscosity is to the working viscosity value, film with the ZBQ-4 coating device, after 180 ℃ of 1h of baking oven baking solidify, obtain high temperature resistant printing ink coating; The Performance Detection situation of printing ink coating that gained is high temperature resistant is as shown in table 1.
Embodiment 3
1) get the good synthetic materials of 65g polyester modified organic silicon resin KE561(Guangzhou Kang Gu company limited), 30g Tiona-RCL69 titanium dioxide (the grand industry of Shanghai well), 2g glass powder, the 2g mica powder, 3g DBE(dicarboxylic acid esters), the 1g isophorone, 0.4g Silok7160 dispersion agent (Si Luoke China operation centre), 0.2g Silok-8144 flow agent (Si Luoke China operation centre), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) get 3g CYMEL303 linking agent (Weng Kaier company limited), the 1g pimelinketone, 0.5g Z-6121 coupling agent (DOW CORNING), 1g A187 coupling agent, 0.4g TEGO628 dispersion agent (the high auxiliary agent of enlightening), 0.1g Silok-8244 flow agent (Si Luoke China operation centre), 0.05g AFCONA2022 defoamer (dust husband Kona chemistry), add in host, filter discharging after dispersion 30min under the 1500rpm rotating speed and obtain ink product;
3) by the high temperature resistant touch screen printing ink prepared, add high temperature resistant touch screen ink by weight 8% mixed diluent (mixed diluent by dicarboxylic acid esters, No. 200 solvent oils and pimelinketone in mass ratio 1:1:1 be mixed to get) dilution, adjusting viscosity is to the working viscosity value, film with the ZBQ-4 coating device, after 250 ℃ of 25min of baking oven baking solidify, obtain high temperature resistant printing ink coating; The Performance Detection situation of printing ink coating that gained is high temperature resistant is as shown in table 1.
Embodiment 4
1) get 65g epoxy modified silicone resin HR-10(Guangzhou Xing Shengjie Science and Technology Ltd.), 27g Tiona595 titanium dioxide (the grand industry of Shanghai well), 5g glass powder, 2g DBE(dicarboxylic acid esters), the 1g200 solvent oil, 0.8g BYK110 dispersion agent (BYK auxiliary agent), 0.1g Silok-8144 flow agent (Si Luoke China operation centre), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) get 3g BL3175 solidifying agent (Bayer Bitterfeld GmbH), 1.2g IPDI solidifying agent (Bayer Bitterfeld GmbH), the 2g pimelinketone, 1.5g Z-6121 coupling agent (DOW CORNING), 0.3g TEGO628 dispersion agent (the high auxiliary agent of enlightening), 0.1g Silok-8244 flow agent (Si Luoke China operation centre), 0.05g AFCONA2022 defoamer (dust husband Kona chemistry), join in host, filter discharging after dispersion 30min and obtain ink product under the 1000rpm rotating speed;
3) by the high temperature resistant touch screen printing ink prepared, add high temperature resistant touch screen ink by weight 5% mixed diluent (mixed diluent by isophorone, dimethylbenzene and pimelinketone in mass ratio 1:1:1 be mixed to get) dilution, adjusting viscosity is to the working viscosity value, film with the ZBQ-4 coating device, after 180 ℃ of 1h of baking oven baking solidify, obtain high temperature resistant printing ink coating; The Performance Detection situation of printing ink coating that gained is high temperature resistant is as shown in table 1.
Embodiment 5
1) get 30g epoxy modified silicone resin HR-10(Guangzhou Xing Shengjie Science and Technology Ltd.), 30g epoxy modified silicone resin SH-023-4(Shenzhen lucky roc fluosilicic Materials Co., Ltd), 25g Tiona595 titanium dioxide (the grand industry of Shanghai well), 8g glass powder, the 4g nano silicon, the 3g mica powder, the 2g isophorone, 0.8g BYK110 dispersion agent (BYK auxiliary agent), 0.2g AFCONA3777s flow agent (dust husband Kona chemistry), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) get 3g IPDI solidifying agent (Bayer Bitterfeld GmbH), 1g dimethylbenzene, the 1g pimelinketone, 1g KH550 coupling agent, 0.6g Silok7160 dispersion agent (Si Luoke China operation centre), 0.05g AFCONA2720 defoamer (dust husband Kona chemistry), join in host, filters discharging after dispersion 30min and obtain ink product under the 1000rpm-1500rpm rotating speed;
3) by the high temperature resistant touch screen printing ink prepared, add high temperature resistant touch screen ink by weight 3% mixed diluent (mixed diluent by isophorone, dimethylbenzene and pimelinketone in mass ratio 1.5:1:1 be mixed to get) dilution, adjusting viscosity is to the working viscosity value, film with the ZBQ-4 coating device, after 180 ℃ of 1h of baking oven baking solidify, obtain high temperature resistant printing ink coating; The Performance Detection situation of printing ink coating that gained is high temperature resistant is as shown in table 1.
The test of table 1 embodiment 1-5 film performance
High temperature resistant touch screen printing ink as shown in table 1, prepared by the present invention, after adding the mixed diluting dilution agent, with the ZBQ-4 coating device, film (touch screen) is on glass, after the baking oven baking-curing, the coating obtained has high temperature resistant 300 ℃ of good tint retentions, flawless, good mechanical properties, sticking power hundred lattice test 0-1 levels, pencil hardness 5H, water-fast, anti-acetone, the etching solution of anti-ITO, acid-proof alkaline is better, and coating is without coming off, without bubble, without variable color; The high temperature resistant touch screen printing ink of a kind of thermoset prepared by the present invention is not limited to the touch screen field, also can be widely used in protection and the decoration of hot parts.
The correlated performance test result of the high temperature resistant touch screen printing ink that table 2 is embodiment 3 preparations.
Table 2 printing ink of the present invention and commercially available prod performance comparison
As shown in table 2, prepared the filming of high temperature resistant touch screen printing ink of the embodiment of the present invention 3 preparations has high temperature resistant 300 ℃ of 100min without xanthochromia, without cracking, hardness is up to 6H, film and there is 0 grade of sticking power, 1 grade of ply adhesion, the reason of the advantage such as chemical reagent resistance and stable mechanical property, mainly higher as silicone content in the modified organic silicone resin of binder, take Si ?O ?Si be main chain, Si ?O key bond energy be 452KJ/mol, Si ?O key polarity large, the alkyl connected on the Si atom is had to the dipole induction, improved the connect stability of alkyl to oxygenizement, at 300 ℃ of lower life-time service, do not decompose, nondiscoloration.Simultaneously, the present invention uses high temperature not xanthochromia crosslinking and curing agent and suitable silane coupling agent, react with the property base ?OH of group alive on modified silicone resin, increase cross-linking density and erect " molecular bridge " between resin and touch screen glass interface, strengthen hardness, endurance and the cohesive strength of resin.
Claims (7)
1. the high temperature resistant touch screen printing ink of thermoset, is characterized in that, in parts by weight, the raw material of its formula consists of:
Described modified organic silicone resin is one or both in polyester modified organic silicon resin and epoxy modified silicone resin;
Described pigment powder is Rutile type Titanium Dioxide and charcoal blacks;
Described dispersion agent is modified polyurethane superpolymer, polyester modification poly phosphate and containing one or more in the interpolymer solution of acidic-group;
Described powder filler is one or more in nano silicon, glass powder, mica powder and talcum powder;
Described thinner is one or more in dicarboxylic acid esters, isophorone, 200 solvent oils, pimelinketone and dimethylbenzene;
Described flow agent is one or more in type siloxane flow agent and non-silicon class flow agent; Described type siloxane flow agent is Silok8144 or Silok8244; Described non-silicon class flow agent is AFCONA3777s or AFCONA3670;
Described defoamer is one or more in modified polyorganosiloxane and non-silicon defoamer; Described modified polyorganosiloxane is AFCONA2022, GSK-716 or SD-100; Described non-silicon defoamer is AFCONA2720;
Described silane coupling agent is one or more in propyl trimethoxy silicane A187, propyl trimethoxy silicane Z6121 and propyl-triethoxysilicane KH550; The described interpolymer solution containing acidic-group is one or more in TEGO628, BYK110 and Silok7160;
Described solidifying agent is one or more in methyl-etherified terpolycyantoamino-formaldehyde resin CYMEL 303 solidifying agent, amino terpolycyantoamino-formaldehyde resin CYMEL 325 solidifying agent and isocyanic ester BL 3175, IPDI solidifying agent;
During preparation, in formulation weight part, get modified organic silicone resin, pigment, powder filler, 0.35-0.95 part dispersion agent, 0.05-0.15 part flow agent and 2-5.4 part mixing diluents, grinding distribution, prepare host; By solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, add in described host after 1-2.6 part mixing diluents stirs, the rear filtration that is uniformly dispersed, and discharging obtains the high temperature resistant touch screen printing ink of thermoset; Described dispersion agent, flow agent and twice consumption sum of thinner are parts by weight in formula material.
2. the high temperature resistant touch screen printing ink of thermoset according to claim 1, is characterized in that, described titanium dioxide is Tupont902
+, one or more in Tiona595 and Tiona RCL69.
3. the high temperature resistant touch screen printing ink of thermoset according to claim 1, is characterized in that, described carbon black is one or more in T1, N330 and TH311.
4. the high temperature resistant touch screen printing ink of thermoset according to claim 1, is characterized in that, described modified polyurethane superpolymer is AFCONA4010 or AFCONA4071; Described polyester modification poly phosphate is AFCONA5010 or AFCONA5210.
5. the high temperature resistant touch screen printing ink of thermoset according to claim 1, is characterized in that, described polyester modified organic silicon resin is JY7200, YS-133 or KE-561.
6. the high temperature resistant touch screen printing ink of thermoset according to claim 1, is characterized in that, described epoxy modified silicone resin is SH-023-4, HR-10 or HG-52.
7. the preparation method of the high temperature resistant touch screen printing ink of the described thermoset of claim 1-6 any one is characterized in that comprising the steps and processing condition:
1) in the composition of raw materials weight part, get modified organic silicone resin, add pigment, powder filler, 0.35-0.95 part dispersion agent, 0.05-0.15 part flow agent, 2-5.4 part thinner, at 2000-2500rpm grinding distribution 1h-1.5h, obtain host;
2) in the composition of raw materials weight part, get solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, 1-2.6 part thinner is in beaker, after stirring, join in described host, under dispersing speed 1000-1500rpm, disperse to filter after 0.5h-1h, discharging obtains the high temperature resistant touch screen printing ink of thermoset;
Described dispersion agent, flow agent and twice consumption sum of thinner are parts by weight in formula material.
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