CN103436094B - High temperature resistant touch screen ink of a kind of thermoset and preparation method thereof - Google Patents
High temperature resistant touch screen ink of a kind of thermoset and preparation method thereof Download PDFInfo
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Abstract
The invention discloses high temperature resistant touch screen ink of a kind of thermoset and preparation method thereof.With weight parts, the raw material of this ink formulations consists of: modified organic silicone resin 55-65 part, titanium dioxide 20-30 part, powder filler 5-15 part, thinner 3-8 part, dispersion agent 0.5-1.4 part, flow agent 0.1-0.3 part, defoamer 0.05-0.1 part, silane coupling agent 1-2 part, solidifying agent 2-5 part.During preparation, 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 obtain host; Solidifying agent, defoamer, silane coupling agent and remaining flow agent, dispersion agent and thinner are added in host, dispersion, filtration, discharging; This ink film is high temperature resistant, and 300 DEG C of high temperature tint retentions are excellent, and on base material, attachment fastness is good, and hardness is high, resistant to acetone wiping, the etching solution of resistance to ITO.
Description
Technical field
The present invention relates to technical field of ink, particularly relate to high temperature resistant touch screen ink of a kind of thermoset and preparation method thereof.
Background technology
Current touch screen is used widely in fields such as smart mobile phone, panel computer, super 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 is engaged in being the core competitiveness place producing touch screen enterprise; Touch screen ink is not only protection and the effect of decoration to touch screen, more directly affects the quality of ITO plated film, has material impact to touch screen sensitivity;
Current commercially available touch screen ink generally uses poly-(ammonia) mechanical property such as ester, epoxy resin and the good resin system of endurance to do ink adhesive, but the easy xanthochromia of coating or cracking after carrying out 280 DEG C of high temperature ITO coating process, the use of the high temperature ITO coating process thus limited, and then limit the further raising of touch screen sensitivity;
The silicone resin of epoxy resin and polyester modification, can combine the thermotolerance of silicone resin excellence and water tolerance with endurance with the mechanical property of epoxy resin, polyester excellence; Zhang Jianhuas etc. adopted in unsaturated polyester post-synthesis phase, and add organosilicon performed polymer, utilize condensation reaction to prepare organosilicon modified polyester, it is thermally-stabilised good, heat decomposition temperature 320 DEG C, and good mechanical properties, is widely applied in solvent-free immersion paint; Tao Zhi waits by force and adopts epoxy resin modified organosilicon, and resin thermal weight loss test (TGA) of preparation shows, completely crued modified resin before 300 DEG C without any weight loss, and good mechanical properties, water tolerance is also better; With this type of modified organic silicone resin as ink adhesive, high temperature resistant tint retention and good mechanical properties, the good touch screen ink of endurance can be prepared;
Summary of the invention
The object of the present invention is to provide a kind of resistance to 300 DEG C to have stable high-temperature performance, tint retention is good, excellent in mechanical performance, and resistant to acetone repeatedly wiping 50 nothings comes off, without the high temperature resistant touch screen ink of thermoset faded.
Another object of the present invention is providing the preparation method of the high temperature resistant touch screen ink of a kind of described thermoset.
Object of the present invention realizes by following technical solution:
The high temperature resistant touch screen ink of a kind of thermoset, with weight parts, 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 be modified polyurethane superpolymer, polyester modification poly phosphate and containing acidic-group interpolymer solution in one or more;
Described powder filler is one or more in nano silicon, glass powder, mica powder and talcum powder;
Described thinner is 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, prepares host; By solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, adds after 1-2.6 part mixing diluents stirs in described host, and filter after being uniformly dispersed, namely discharging obtains the high temperature resistant touch screen ink of thermoset; Described dispersion agent, flow agent and thinner twice consumption sum is parts by weight in formula material.
For realizing the object of the invention further, 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 ink, comprises the steps and processing condition:
1) with composition of raw materials parts by weight, 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) with composition of raw materials parts by weight, 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, join in described host after stirring, filter disperse 0.5h-1h under dispersing speed 1000-1500rpm after, namely discharging obtains the high temperature resistant touch screen ink of thermoset;
Described dispersion agent, flow agent and thinner twice consumption sum is parts by weight in formula material.
Comprise the steps: during touch screen ink use that this thermoset is high temperature resistant
1) the high temperature resistant touch screen ink will 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 is applicable to viscosity number to construction;
2) use ZBQ-4 coating device at base material (glass, tinplate etc.) film, toast after 180 DEG C of-200 DEG C of 1h or 250 DEG C of 25min solidifications through baking oven and obtain high temperature resistant ink coating;
Relative to prior art, tool of the present invention has the following advantages:
1) the high temperature resistant touch screen ink provided, adopt the silicone resin of modification as binder, have good resistance toheat, high temperature resistant 300 DEG C/100min film is complete, and tint retention is good, flawless.
2) hydroxyl on modified organic silicone resin under certain condition, can with the active group cross-linking and curing reaction in solidifying agent, make paint film have tridimensional network, make at glass surface, it has that excellent sticking power, simultaneously hardness of film are high, water-tolerant, that resistant to acetone wiping and ITO etching solution soak paint film is complete;
Embodiment
Be explained in detail the present invention below in conjunction with embodiment, object is in order to the public better understands the content of the present patent application instead of the restriction to technology contents described in the present patent application.Do not violate do in the present patent application invention spirit any increase and decrease, replacement, improvement is all within the present patent application technical scheme required for protection.
Embodiment 1
1) 55 polyester modified organic silicon resin JY7200(Dongguan Jun Yi Chemical Industry Science Co., Ltd are got), 20g Tupont902
+titanium dioxide (E.I.Du Pont Company), 3g glass powder, 2g nano silicon, 1g isophorone, 1g200 solvent oil, 0.3gBYK110 dispersion agent (BYK auxiliary agent), 0.1g AFCONA3670 flow agent (dust husband Kona chemistry), joins in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) 1g CYMEL303 is got, 1g CYMEL325 linking agent (Weng Kaier company limited), 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 and namely obtain ink product under 1000rpm rotating speed after disperseing 30min;
3) the high temperature resistant touch screen ink will 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) dilute, adjusting viscosity is to working viscosity value, with ZBQ-4 coating device film, toast after 180 DEG C of 1h solidifications through baking oven and obtain high temperature resistant ink coating; The Performance Detection situation of gained is high temperature resistant ink coating is as shown in table 1.
Embodiment 2
1) 60g epoxy modified silicone resin HG-52(Zhong Hao Chenguang Research Institute of Chemical Industry company limited is got), 10gTiona-RCL69 titanium dioxide (the grand industry of Shanghai well), 15g Tiona-595 titanium dioxide (the grand industry of Shanghai well), 5g glass powder, 2g nano silicon, 1g talcum powder, 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) 2.25g CYMEL325 linking agent (Weng Kaier company limited) is got, 2g DBE(dicarboxylic acid esters), 1g A-187 coupling agent, 1g KH550 coupling agent, 0.3g TEGO-628 dispersion agent (enlightening height auxiliary agent), 0.1g AFCONA3670 flow agent (dust husband Kona chemistry), 0.05g GSK-716 defoamer (Gauss enters fine chemistry industry), join in host, filter discharging after disperseing 30min under 1200rpm rotating speed and namely obtain ink product;
3) the high temperature resistant touch screen ink will 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) dilute, adjusting viscosity is to working viscosity value, with ZBQ-4 coating device film, toast after 180 DEG C of 1h solidifications through baking oven and obtain high temperature resistant ink coating; The Performance Detection situation of gained is high temperature resistant ink coating is as shown in table 1.
Embodiment 3
1) the good synthetic materials company limited of 65g polyester modified organic silicon resin KE561(Guangzhou Kang Gu is got), 30gTiona-RCL69 titanium dioxide (the grand industry of Shanghai well), 2g glass powder, 2g mica powder, 3g DBE(dicarboxylic acid esters), 1g isophorone, 0.4g Silok7160 dispersion agent (operation centre of Si Luoke China), 0.2g Silok-8144 flow agent (operation centre of Si Luoke China), join in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) 3g CYMEL303 linking agent (Weng Kaier company limited) is got, 1g pimelinketone, 0.5g Z-6121 coupling agent (DOW CORNING), 1g A187 coupling agent, 0.4g TEGO628 dispersion agent (enlightening height auxiliary agent), 0.1g Silok-8244 flow agent (operation centre of Si Luoke China), 0.05g AFCONA2022 defoamer (dust husband Kona chemistry), add in host, filter discharging after disperseing 30min under 1500rpm rotating speed and namely obtain ink product;
3) the high temperature resistant touch screen ink will 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) dilute, adjusting viscosity is to working viscosity value, with ZBQ-4 coating device film, toast after 250 DEG C of 25min solidifications through baking oven and obtain high temperature resistant ink coating; The Performance Detection situation of gained is high temperature resistant ink coating is as shown in table 1.
Embodiment 4
1) 65g epoxy modified silicone resin HR-10(Guangzhou Xing Shengjie Science and Technology Ltd. is got), 27g Tiona595 titanium dioxide (the grand industry of Shanghai well), 5g glass powder, 2g DBE(dicarboxylic acid esters), 1g200 solvent oil, 0.8g BYK110 dispersion agent (BYK auxiliary agent), 0.1g Silok-8144 flow agent (operation centre of Si Luoke China), joins in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) 3g BL3175 solidifying agent (Bayer Bitterfeld GmbH) is got, 1.2g IPDI solidifying agent (Bayer Bitterfeld GmbH), 2g pimelinketone, 1.5gZ-6121 coupling agent (DOW CORNING), 0.3g TEGO628 dispersion agent (enlightening height auxiliary agent), 0.1g Silok-8244 flow agent (operation centre of Si Luoke China), 0.05g AFCONA2022 defoamer (dust husband Kona chemistry), join in host, filter discharging disperse 30min under 1000rpm rotating speed after and namely obtain ink product;
3) the high temperature resistant touch screen ink will 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 working viscosity value, with ZBQ-4 coating device film, toast after 180 DEG C of 1h solidifications through baking oven and obtain high temperature resistant ink coating; The Performance Detection situation of gained is high temperature resistant ink coating is as shown in table 1.
Embodiment 5
1) 30g epoxy modified silicone resin HR-10(Guangzhou Xing Shengjie Science and Technology Ltd. is got), 30g epoxy modified silicone resin SH-023-4(Shenzhen Ji Peng fluosilicic Materials Co., Ltd), 25g Tiona595 titanium dioxide (the grand industry of Shanghai well), 8g glass powder, 4g nano silicon, 3g mica powder, 2g isophorone, 0.8g BYK110 dispersion agent (BYK auxiliary agent), 0.2g AFCONA3777s flow agent (dust husband Kona chemistry), joins in dispersion tank, after stirring, after shredder 2500rpm grinding distribution 90min, filter and obtain host;
2) 3g IPDI solidifying agent (Bayer Bitterfeld GmbH) is got, 1g dimethylbenzene, 1g pimelinketone, 1g KH550 coupling agent, 0.6g Silok7160 dispersion agent (operation centre of Si Luoke China), 0.05g AFCONA2720 defoamer (dust husband Kona chemistry), joins in host, filters discharging and namely obtain ink product under 1000rpm-1500rpm rotating speed after disperseing 30min;
3) the high temperature resistant touch screen ink will 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 working viscosity value, with ZBQ-4 coating device film, toast after 180 DEG C of 1h solidifications through baking oven and obtain high temperature resistant ink coating; The Performance Detection situation of gained is high temperature resistant ink coating is as shown in table 1.
Table 1 embodiment 1-5 film performance is tested
As shown in table 1, high temperature resistant touch screen ink prepared by the present invention, after adding mixed diluting dilution agent, with ZBQ-4 coating device film on (touch screen) glass, after baking oven baking-curing, the coating obtained has high temperature resistant 300 DEG C of good tint retentions, flawless, good mechanical properties, sticking power hundred lattice test 0-1 level, pencil hardness 5H, water-fast, resistant to acetone, the etching solution of resistance to ITO, acid-proof alkaline is better, and coating is without coming off, bubble-free, without variable color; A kind of thermoset prepared by the present invention is high temperature resistant, and touch screen ink is not limited to touch screen field, also can be widely used in protection and the decoration of hot parts.
Table 2 is the correlated performance test result of high temperature resistant touch screen ink prepared by embodiment 3.
Table 2 ink of the present invention and commercially available prod performance comparison
As shown in table 2, film obtained by high temperature resistant touch screen ink prepared by the embodiment of the present invention 3 has high temperature resistant 300 DEG C of 100min without xanthochromia, without cracking, hardness is up to 6H, film has sticking power 0 grade, ply adhesion 1 grade, 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, with Si ?O ?Si for main chain, Si ?O key bond energy be 452KJ/mol, Si ?O key polarity large, dipole is had to respond to the alkyl that Si atom connects, improve the stability of connected alkyl to oxygenizement, at 300 DEG C, life-time service does not decompose, nondiscoloration.Simultaneously, the present invention uses high temperature non yellowing crosslinking and curing agent and suitable silane coupling agent, roll into a ball ?OH with the property base alive on modified silicone resin to react, increase cross-linking density and erect " molecular bridge " between resin and touch screen glass interface, strengthen the hardness of resin, endurance and cohesive strength.
Claims (5)
1. the high temperature resistant touch screen ink of thermoset, is characterized in that, with weight parts, 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 polyester modified organic silicon resin is JY7200; Described epoxy modified silicone resin is SH-023-4, HR-10 or HG-52;
Described pigment powder is Rutile type Titanium Dioxide and charcoal blacks;
Described dispersion agent be modified polyurethane superpolymer, polyester modification poly phosphate and containing acidic-group interpolymer solution in one or more;
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 non-silicon defoamer; 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 isocyanic ester BL 3175 and 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, prepares host; By solidifying agent, defoamer, silane coupling agent, 0.05-0.15 part flow agent, 0.15-0.45 part dispersion agent, adds after 1-2.6 part mixing diluents stirs in described host, and filter after being uniformly dispersed, namely discharging obtains the high temperature resistant touch screen ink of thermoset; Described dispersion agent, flow agent and thinner twice consumption sum is parts by weight in formula material.
2. the high temperature resistant touch screen ink of thermoset according to claim 1, is characterized in that, described titanium dioxide is one or more in Tiona595 and Tiona RCL69.
3. the high temperature resistant touch screen 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 ink of thermoset according to claim 1, it is characterized in that, described modified polyurethane superpolymer is AFCONA4010 or AFCONA4071; Described polyester modification poly phosphate is AFCONA5010.
5. the preparation method of the high temperature resistant touch screen ink of thermoset described in any one of claim 1-4, is characterized in that comprising the steps and processing condition:
1) with composition of raw materials parts by weight, 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) with composition of raw materials parts by weight, 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, join in described host after stirring, filter disperse 0.5h-1h under dispersing speed 1000-1500rpm after, namely discharging obtains the high temperature resistant touch screen ink of thermoset;
Described dispersion agent, flow agent and thinner twice consumption sum is parts by weight in formula material.
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| CN103013225A (en) * | 2012-12-25 | 2013-04-03 | 广州慧谷工程材料有限公司 | IML gloss oil and IML printing ink and preparation method and application thereof |
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| CN102719191A (en) * | 2012-06-26 | 2012-10-10 | 华南理工大学 | High-temperature-resistant anticorrosive paint and preparation method thereof |
| CN103013225A (en) * | 2012-12-25 | 2013-04-03 | 广州慧谷工程材料有限公司 | IML gloss oil and IML printing ink and preparation method and application thereof |
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