CN107129584A - A kind of preparation method of PEDOT/PSS aqueous dispersions and the antistatic coating prepared with the aqueous dispersion - Google Patents
A kind of preparation method of PEDOT/PSS aqueous dispersions and the antistatic coating prepared with the aqueous dispersion Download PDFInfo
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- CN107129584A CN107129584A CN201710331769.5A CN201710331769A CN107129584A CN 107129584 A CN107129584 A CN 107129584A CN 201710331769 A CN201710331769 A CN 201710331769A CN 107129584 A CN107129584 A CN 107129584A
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Abstract
The invention discloses a kind of preparation method of PEDOT/PSS aqueous dispersions, and the aqueous heat-setting solvent-resisting antistatic coating prepared using PEDOT/PSS aqueous dispersions, the coating includes the raw material of following mass fractions:50 65 parts of PEDOT/PSS aqueous dispersions, 24 34 parts of waterborne polyurethane resin, 0.25 0.5 parts of coupling agent, 0.01 0.2 parts of crosslinking agent, 10 15 parts of cosolvent, 0.1 0.4 parts of additive.The coating adhesion that the antistatic coating of the present invention coats formation on glass is strong, and hardening time is short, while solvent resistant wiping ability is strong.
Description
Technical field
The present invention relates to a kind of polymer-function material field, and in particular to a kind of preparation of PEDOT/PSS aqueous dispersions
Method and the antistatic coating prepared with the aqueous dispersion.
Background technology
Electrostatic can produce certain harm to daily life and production.Produced during the production and use of electronic component
Electrostatic can electron manufacturing industry bring huge economic loss.For example, can shape in the electric charge that insulated electronic element surface is accumulated
Into electric field, simultaneously adsorption of dust causes short circuit;The accumulation of Flied emission semiconductor electrostatic is likely to result in current loop, produced by electric charge
When voltage is more than the breakdown voltage of transistor dielectric layer, dielectric layer can be caused to damage.It is antistatic with the development of electronics manufacturing
Technology is also badly in need of fast development.
It is poly-(3,4- ethene dioxythiophenes)/ poly-(Styrene sulfonic acid), referred to as(PEDOT/PSS)It is several commercially viable at present
In the conducting polymer of production, uniquely high transmission rate and the raw material of low resistance can be ensured simultaneously to a certain extent, the material
To develop a kind of one of quick and most valued conducting polymer in recent years.PEDOT/PSS aqueous dispersions are in antistatic coating
Middle acquisition immense success.For example, Publication No. CN102731971A and CN104650545A patent of invention disclose highly conductive
The preparation method of rate PEDOT/PSS aqueous dispersions;Publication No. CN103865364A, CN103237852A and CN104211969A
Patent of invention disclose preparation method and application of the PEDOT/PSS aqueous dispersions in antistatic coating;Publication No.
CN101643549A and CN103302876A patent of invention individually discloses a kind of manufacture method of antistatic coating and continuous
Production technology;Publication No. CN102476490A, CN103173108A, CN104194580A and CN104946124A invention are special
Profit discloses the stability approach for improving PEDOT/PSS antistatic coatings;Publication No. CN104893538A patent of invention is public
A kind of preparation method of sulfonated graphene/PEDOT aqueous dispersions and the application in antistatic coating are opened;Publication No.
CN103881537A and CN103788859A patent of invention discloses photocuring PEDOT/PSS antistatic coatings.Above-mentioned patent
The antistatic coating common problem of announcement is that the solvent resistant of antistatic coating wipes ability, and hardening time is long, no
Beneficial to large-scale production.
The content of the invention
For above-mentioned problems of the prior art, the present invention provides a kind of PEDOT/PSS aqueous dispersions, and uses the water
Antistatic coating prepared by dispersion, the coating adhesion that antistatic coating coats formation on glass is strong, and hardening time is short, together
When solvent resistant wipe ability it is strong.
Above-mentioned purpose is realized by following proposal:
A kind of preparation method of PEDOT/PSS aqueous dispersions, it is characterised in that methods described in turn includes the following steps, wherein
The amount of raw material is in mass:
(1)By 25-35 parts of kayexalates and 0.75-0.9 parts of DBSAs be added to 2000-3600 parts go from
In sub- water, solution is formed;
(2)To step(1)In solution in add concentrated hydrochloric acid, make solution pH be 1.5-2.0, thereto add 10 parts 3,4-
Ethylenedioxy thiophene, high-speed stirred 2 hours, form reaction solution at room temperature;
(3)By 22 parts of ammonium persulfates and 6 parts of ferric sulfate solutions in 400-600 parts of deionized waters, mixed liquor is formed, the mixing is molten
Liquid is added dropwise to step(3)Reaction solution in, the time used in dropping liquid be 1 hour;
(4)Reaction solution high-speed stirred 5 hours at room temperature after dropping liquid will be completed, add total number for 120-2200 parts the moon,
After resin cation, it is slowly stirred 10 hours;
(5)Resin is filtered out, filtrate is obtained, filtrate is obtained into PEDOT/ in homogeneous under 100MPa 10 times with high pressure homogenizer
PSS aqueous dispersions.
A kind of aqueous heat-setting solvent-resisting prepared using above-mentioned PEDOT/PSS aqueous dispersions is antistatic to be applied
Material, it is characterised in that the coating includes the raw material of following mass fractions:It is 50-65 parts of PEDOT/PSS aqueous dispersions, aqueous poly-
24-34 parts of urethane resin, 0.25-0.5 parts of coupling agent, 0.01-0.2 parts of crosslinking agent, 10-15 parts of cosolvent, additive 0.1-0.4
Part.
According to above-mentioned antistatic coating, it is characterised in that the waterborne polyurethane resin is Sancure825, RU-71-
One or more in 035 and XR-28-404.
According to above-mentioned antistatic coating, it is characterised in that the crosslinking agent be aziridine crosslinker, including XAMA-7,
One or more in QL-GWD-D2 and QL-A2000-CX.
According to above-mentioned antistatic coating, it is characterised in that the coupling agent is one kind in TX-100, KH560 and KH570
Or it is several.
According to above-mentioned antistatic coating, it is characterised in that the cosolvent is one or both of DMSO and EG.
According to above-mentioned antistatic coating, it is characterised in that the additive be it is a kind of in imidazoles and 2-methylimidazole or
Two kinds.
A kind of preparation method of above-mentioned antistatic coating, it is characterised in that by the PEDOT/PSS aqueous dispersions, water
Property polyurethane resin, coupling agent, cosolvent, additive mix in proportion, be stirred at room temperature 2 hours, add the crosslinking agent,
Stir, obtain described antistatic coating.
A kind of preparation method of the antistatic coating prepared using above-mentioned antistatic coating, it is characterised in that the side
Method comprises the following steps successively:
(1)By isopropyl alcohol and water by volume 1:1 mixing, is made mixed solvent, and described coating is dilute with the mixed solvent
Release 10 times;
(2)By step(1)Coating after middle dilution is coated in PET or glass baseplate with bar, at 110 DEG C dry 1
Minute, that is, obtain the antistatic coating.
Beneficial effects of the present invention:
Compared with prior art, the advantage of the invention is that:The present invention is using PEDOT/PSS as conductive component, with aqueous poly- ammonia
Ester resin is matrix resin, adds coupling agent, crosslinking agent, cosolvent and additive, and preparing solvent resistant by heat cure wipes
The antistatic coating wiped.The coating adhesion that formation is coated on glass is strong, and sheet resistance is 104 ~ 106 Ω/, light transmittance >
98%, good weatherability is wiped 200 times, coating surface resistance is maintained at 105 ~ 108 Ω/ with ethanol or toluene.
Embodiment
The preparation of PEDOT/PSS aqueous dispersions in turn includes the following steps, and wherein the amount of raw material is in mass:
(1)By 25-35 parts of kayexalates and 0.75-0.9 parts of DBSAs be added to 2000-3600 parts go from
In sub- water, solution is formed;
(2)To step(1)In solution in add concentrated hydrochloric acid, make solution pH be 1.5-2.0, thereto add 10 parts of 3,4- second
Dioxy thiophene is supportted, at room temperature high-speed stirred 2 hours, form reaction solution;
(3)By 22 parts of ammonium persulfates and 6 parts of ferric sulfate solutions in 400-600 parts of deionized waters, mixed liquor is formed, by mixed solution
It is added dropwise to step(3)Reaction solution in, the time used in dropping liquid be 1 hour;
(4)Reaction solution high-speed stirred 5 hours at room temperature after dropping liquid will be completed, add total number for 120-2200 parts the moon,
After resin cation, it is slowly stirred 10 hours;
(5)Resin is filtered out, filtrate is obtained, filtrate is obtained into PEDOT/ in homogeneous under 100MPa 10 times with high pressure homogenizer
PSS aqueous dispersions.
The aqueous heat-setting solvent-resisting antistatic coating of the present invention includes the raw material of following mass fractions:
50-65 parts of PEDOT/PSS aqueous dispersions, 24-34 parts of waterborne polyurethane resin, 0.25-0.5 parts of coupling agent, crosslinking agent 0.01-
0.2 part, 10-15 parts of cosolvent, 0.1-0.4 parts of additive.Wherein, waterborne polyurethane resin is Germany Lu Borun's
One or more in Sancure825, RU-71-035 and XR-28-404, Sancure825 is German Lubrizol Corp.'s production
Waterborne polyurethane resin, RU-71-035 and XR-28-404 are the fine coating of this tal fibre(Suzhou)It is aqueous that Co., Ltd produces
Polyurethane resin;Crosslinking agent is aziridine crosslinker, including XAMA-7, QL-GWD-D2 and QL-A2000-CX one or more of,
Wherein, XAMA-7 is the aziridine crosslinker that Bayer A.G produces, and QL-GWD-D2 and QL-A2000-CX are that Wuhan is imperial by force
The aziridine crosslinker of new chemical materialses Co., Ltd production;Coupling agent is one or more in TX-100, KH560 and KH570,
Wherein, TX-100 is Sigma-Aldrich(Sigma-Aldrich)The coupling agent of production, KH560 and KH570 are the resistance to Jilin Chemical of peace
The coupling agent of company production;Cosolvent is DMSO(Dimethyl sulfoxide (DMSO))And EG(Ethylene glycol)One or both of;Additive
For one or two in imidazoles and 2-methylimidazole.
PEDOT/PSS aqueous dispersions, waterborne polyurethane resin, coupling agent, cosolvent, additive are mixed in proportion,
Stir 2 hours at room temperature, add crosslinking agent, stir, you can obtain antistatic coating.
The antistatic coating of the present invention when in use, by isopropyl alcohol and water by volume 1:1 mixing, is made mixed solvent,
Antistatic coating is diluted 10 times with mixed solvent, then the coating after dilution is coated in PET or glass baseplate with bar
On, in being dried 1 minute at 110 DEG C, that is, obtain antistatic coating.
The present invention is further detailed with specific embodiment below.
Embodiment 1
It is accurate to weigh 30 parts of kayexalates and 0.9 part of DBSA, add in 3600 parts of deionized waters, formed
Solution.Using concentrated hydrochloric acid, regulation pH value of solution is 1.5, thereto the middle 3,4-ethylene dioxythiophene room temperature high-speed stirring for adding 10 parts
2h is mixed, reaction solution is formed.By 22 parts of ammonium persulfates and 6 parts of ferric sulfate solutions in 400 parts of deionized waters, by the mixed solution dropwise
Add in reaction solution, 1h completion of dropping, room temperature high-speed stirred 5h, add each 200 parts of anions and canons resin, 300rpm stirrings 10
Hour, resin is filtered out, filtrate is obtained into neutral PEDOT/PSS aqueous dispersions in homogeneous under 100MPa 10 times with high pressure homogenizer.
Embodiment 2
Accurately weigh 65% PEDOT/PSS aqueous dispersions, 24.4% waterborne polyurethane resin prepared by embodiment 1
(Sancure825), 0.25%KH560,8%DMSO, 2%EG and 0.15% imidazoles be added in beaker, and 2h, 0.2% is stirred at room temperature
XAMA-7 is added in above-mentioned solution, stirs and neutral antistatic coating is made.Gained aqueous coating and isopropanol are mixed
Solvent(1:1 V/V)After 10 times of dilution, it is coated on 8 μm of bars on quartz glass, 1min is dried at 110 DEG C, visible light wave is used
Section light transmittance instrument test light transmittance is 98.2%, and it is 2.5 × 10 that sheet resistance is measured with surface resistivity instrument6Ω/□.Use ethanol
Wipe 200 times, measurement surface resistance is 2.1 × 10 again7Ω/□.With toluene wipe 200 times, again measurement surface resistance be
8.7×106Ω/, 1 month in air, coating surface resistance 1.4 × 108Ω/□。
Embodiment 3:
Accurately weigh 65% PEDOT/PSS aqueous dispersions, 24.5% waterborne polyurethane resin prepared by embodiment 1(RU-71-
035), 0.25%KH560,10%DMSO and 0.10% imidazoles be added in beaker, and 2h is stirred at room temperature, and 0.15%XAMA-7 adds above-mentioned
In solution, stir and neutral antistatic coating is made.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)It is dilute
Release after 10 times, be coated on 8 μm of bars on PET, 1min is dried at 110 DEG C, light transmittance is tested with visible light wave range light transmittance instrument
For 98.4%, it is 1.0 × 10 that sheet resistance is measured with surface resistivity instrument6Ω/□.With ethanol 200 times, measurement table again
Surface resistance is 3.6 × 107Ω/□.Wiped 200 times with toluene, measurement surface resistance is 2.7 × 10 again7Ω/, exposed to sky
1 month in gas, coating surface resistance 2.2 × 108Ω/□。
Embodiment 4:
Accurate weigh prepares 50% PEDOT/PSS aqueous dispersions, 34.5% waterborne polyurethane resin by embodiment 1(XR-28-
404), 0.25%KH560,15%DMSO and 0.10% imidazoles be added in beaker, and 2h is stirred at room temperature, and 0.15%XAMA-7 adds above-mentioned
In solution, stir and neutral antistatic coating is made.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)It is dilute
Release after 10 times, be coated on 8 μm of bars on quartz glass, 1min is dried at 110 DEG C, test saturating with visible light wave range light transmittance instrument
Light rate is 98.5%, and it is 6.6 × 10 that sheet resistance is measured with surface resistivity instrument6Ω/□.With ethanol 200 times, survey again
Scale surface resistance is 5.6 × 108Ω/□.Wiped 200 times with toluene, measurement surface resistance is 5.7 × 10 again8Ω/, exposure
1 month in air, coating surface resistance 9.0 × 108Ω/□。
Embodiment 5
It is accurate to weigh in 25 parts of kayexalates and 0.78 part of DBSA 3000 parts of deionized water of addition, shape
Into solution.Concentrated hydrochloric acid regulation pH value of solution is 1.5, thereto the 3,4-ethylene dioxythiophene of 10 parts of addition, room temperature high-speed stirred 2h,
Form reaction solution.By 22 parts of ammonium persulfates and 6 parts of ferric sulfate solutions in 600 parts of deionized waters, mixed solution is formed, will be mixed molten
Liquid is added dropwise in reaction solution, 1h completion of dropping, room temperature high-speed stirred 5h, adds each 200 parts of anions and canons resin, 300rpm
Stirring 10 hours, filters out resin, and filtrate is obtained into neutral PEDOT/PSS water in homogeneous under 100MPa 10 times with high pressure homogenizer
Dispersion.
Embodiment 6
Accurately weigh 65% PEDOT/PSS aqueous dispersions, 6.1% waterborne polyurethane resin prepared by embodiment 5
(Sancure825), 18.3% waterborne polyurethane resin RU-71-035,0.25%KH560,7.5%DMSO, 2.5%EG and 0.15% miaow
Azoles is added in beaker, and 2h is stirred at room temperature, and 0.2%XAMA-7 is added in above-mentioned solution, stirs and neutral antistatic painting is made
Material.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)After 10 times of dilution, it is coated on 8 μm of bars on PET, 110
1min is dried at DEG C, is 98.0% with visible light wave range light transmittance instrument test light transmittance, sheet resistance is measured with surface resistivity instrument
For 8.9 × 104Ω/□.With ethanol 200 times, measurement surface resistance is 1.1 × 10 again6Ω/□.200 are wiped with toluene
Secondary, measurement surface resistance is 7.0 × 10 again5Ω/, 1 month in air, coating surface resistance 2.4 × 106Ω/
□。
Embodiment 7
Accurately weigh 50% PEDOT/PSS aqueous dispersions, 9.4% waterborne polyurethane resin prepared by embodiment 5
(Sancure825), 28.0% waterborne polyurethane resin RU-71-035,0.25%KH560,10%DMSO, 2.0%EG and 0.15% miaow
Azoles is added in beaker, and 2h is stirred at room temperature, and 0.2%XAMA-7 is added in above-mentioned solution, stirs and neutral antistatic painting is made
Material.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)After 10 times of dilution, it is coated on 8 μm of bars on PET, 110
1min is dried at DEG C, is 98.0% with visible light wave range light transmittance instrument test light transmittance, sheet resistance is measured with surface resistivity instrument
For 5.7 × 105Ω/□.With ethanol 200 times, measurement surface resistance is 4.1 × 10 again6Ω/□.200 are wiped with toluene
Secondary, measurement surface resistance is 6.5 × 10 again6Ω/, 1 month in air, coating surface resistance 8.4 × 106Ω/
□。
Embodiment 8
Accurately weigh 50% PEDOT/PSS aqueous dispersions, 9.1% waterborne polyurethane resin prepared by embodiment 5
(Sancure825), 27.3% waterborne polyurethane resin RU-71-035,0.25%KH560,12%DMSO, 1.0%EG and 0.15% miaow
Azoles is added in beaker, is stirred at room temperature on 2h, 0.12%XAMA-7,0.05% QL-GWD-D2,0.03%QL-A2000-CX addition
State in solution, stir and neutral antistatic coating is made.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)
After 10 times of dilution, it is coated on 8 μm of bars on PET, 1min is dried at 110 DEG C, printing opacity is tested with visible light wave range light transmittance instrument
Rate is 98.1%, and it is 1.1 × 10 that sheet resistance is measured with surface resistivity instrument5Ω/□.With ethanol 200 times, measure again
Sheet resistance is 3.1 × 106Ω/□.Wiped 200 times with toluene, measurement surface resistance is 4.9 × 10 again6Ω/, is exposed to
1 month in air, coating surface resistance 8.0 × 107Ω/□。
Embodiment 9
Accurately weigh 65% PEDOT/PSS aqueous dispersions, 24.6% waterborne polyurethane resin prepared by embodiment 1
(Sancure825), 0.25%KH560,8%DMSO, 2%EG and 0.15% imidazoles be added in beaker, is stirred at room temperature during 2h is made
Property antistatic coating.By gained aqueous coating and isopropyl alcohol mixed solvent(1:1 V/V)After 10 times of dilution, coated with 8 μm of bars
In on quartz glass, 1min is dried at 110 DEG C, is 98.3% with visible light wave range light transmittance instrument test light transmittance, uses sheet resistance
It is 1.7 × 10 that rate instrument, which measures sheet resistance,5Ω/□.Wiped 200 times with ethanol 200 times or with toluene, nonreactive electrostatic energy
Power, 1 month in air, coating surface resistance 7.1 × 106Ω/□。
Embodiment 10
Accurately weigh 65% PEDOT/PSS aqueous dispersions, 6.1% waterborne polyurethane resin prepared by embodiment 5
(Sancure825), 18.3% waterborne polyurethane resin RU-71-035,0.25%KH560,7.5%DMSO, 2.5%EG and 0.15% miaow
Azoles, which is added in beaker, is stirred at room temperature the i.e. obtained neutral antistatic coatings of 2h.By gained aqueous coating and isopropyl alcohol mixed solvent
(1:1 V/V)After 10 times of dilution, it is coated on 8 μm of bars on PET, 1min is dried at 110 DEG C, with visible light wave range light transmittance instrument
It is 98.5% to test light transmittance, and it is 2.1 × 10 that sheet resistance is measured with surface resistivity instrument4Ω/□.With ethanol or toluene
Wipe 200 times, no antistatic effect, 1 month in air, coating surface resistance 1.3 × 106Ω/□。
Claims (9)
1. a kind of preparation method of PEDOT/PSS aqueous dispersions, it is characterised in that methods described in turn includes the following steps, its
The amount of middle raw material is in mass:
(1)By 25-35 parts of kayexalates and 0.75-0.9 parts of DBSAs be added to 2000-3600 parts go from
In sub- water, solution is formed;
(2)To step(1)In solution in add concentrated hydrochloric acid, make solution pH be 1.5-2.0, thereto add 10 parts 3,4-
Ethylenedioxy thiophene, high-speed stirred 2 hours, form reaction solution at room temperature;
(3)By 22 parts of ammonium persulfates and 6 parts of ferric sulfate solutions in 400-600 parts of deionized waters, mixed liquor is formed, the mixing is molten
Liquid is added dropwise to step(3)Reaction solution in, the time used in dropping liquid be 1 hour;
(4)Reaction solution high-speed stirred 5 hours at room temperature after dropping liquid will be completed, add total number for 120-2200 parts the moon,
After resin cation, it is slowly stirred 10 hours;
(5)Resin is filtered out, filtrate is obtained, filtrate is obtained into PEDOT/ in homogeneous under 100MPa 10 times with high pressure homogenizer
PSS aqueous dispersions.
2. aqueous heat-setting solvent-resisting prepared by the PEDOT/PSS aqueous dispersions described in a kind of usage right requirement 1 resists
Electrostatic coatings, it is characterised in that the coating includes the raw material of following mass fractions:50-65 parts of PEDOT/PSS aqueous dispersions,
24-34 parts of waterborne polyurethane resin, 0.25-0.5 parts of coupling agent, 0.01-0.2 parts of crosslinking agent, 10-15 parts of cosolvent, additive
0.1-0.4 parts.
3. antistatic coating according to claim 2, it is characterised in that the waterborne polyurethane resin is
One or more in Sancure825, RU-71-035 and XR-28-404.
4. antistatic coating according to claim 2, it is characterised in that the crosslinking agent is aziridine crosslinker, including
One or more in XAMA-7, QL-GWD-D2 and QL-A2000-CX.
5. antistatic coating according to claim 2, it is characterised in that the coupling agent be TX-100, KH560 and
It is one or more of in KH570.
6. antistatic coating according to claim 2, it is characterised in that the cosolvent be one kind in DMSO and EG or
Two kinds.
7. antistatic coating according to claim 2, it is characterised in that the additive is in imidazoles and 2-methylimidazole
It is one or two kinds of.
8. the preparation method of the antistatic coating described in a kind of claim 2, it is characterised in that by the PEDOT/PSS moisture
Granular media, waterborne polyurethane resin, coupling agent, cosolvent, additive are mixed in proportion, are stirred at room temperature 2 hours, are added described
Crosslinking agent, stirs, and obtains described antistatic coating.
9. the preparation method of antistatic coating prepared by the antistatic coating described in a kind of usage right requirement 2, it is characterised in that
Methods described comprises the following steps successively:
(1)By isopropyl alcohol and water by volume 1:1 mixing, is made mixed solvent, and described coating is dilute with the mixed solvent
Release 10 times;
(2)By step(1)Coating after middle dilution is coated in PET or glass baseplate with bar, at 110 DEG C dry 1
Minute, that is, obtain the antistatic coating.
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CN108777187A (en) * | 2018-05-29 | 2018-11-09 | 成都莫比斯科技有限公司 | A method of it improving PEDOT conductive films adhesive force and scratch resistance can |
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CN116120820A (en) * | 2021-11-12 | 2023-05-16 | 株式会社爱帛 | Coating composition, method for producing same, protective film, optical film, and display device |
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