CN104629611A - Method for preparing light-curing conductive coating - Google Patents
Method for preparing light-curing conductive coating Download PDFInfo
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- CN104629611A CN104629611A CN201310565790.3A CN201310565790A CN104629611A CN 104629611 A CN104629611 A CN 104629611A CN 201310565790 A CN201310565790 A CN 201310565790A CN 104629611 A CN104629611 A CN 104629611A
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Abstract
The invention relates to a method for preparing a light-curing conductive coating. The method comprises the following steps: synthesizing a sulfonate type polyurethane resin prepolymer by using polycarbonate diol (PCDL2000), isophorone diisocyanate (IPDI), 1,4- butanediol (BDO), N, N-bis(2-hydroxyethyl)-2-amino sodium ethanesulfonic acid and hydroxyethyl methacrylate (HEMA) as raw materials, and then chemically reacting with 3,4-ethylenedioxythiophene to be prepared into intrinsic conductive resin; simultaneously preparing graphene-polypyrrole conductive nano-powder by an in-situ polymerization method, mixing with the intrinsic conductive resin to react, and adding a reactive diluent, a light initiator and the like to be prepared into the light-curing conductive coating. The conductive coating can be quickly cured to form a film by UV irradiation, has superior mechanical properties and good electrical conductivity, and can be widely applied to the fields of monitors, electrical appliances, communication equipment, electronic products and the like.
Description
Technical field
A preparation method for light curable conductive coating, belongs to ultraviolet-curing paint field.
Background technology
Electrically conducting coating is the special functional coating developed rapidly with modern science and technology.In recent years, electrically conducting coating is applied in the multiple military, civilian industrial circles such as electronics, electrical equipment, aviation, chemical industry, printing.The coating that electrically conducting coating can use as electrical conductor, as: hybrid integrated circuit, printed-wiring board (PWB), keyboard switch, the heating paint of warming and vehicle glass frost prevention, anti-fouling ship paint etc.; Can as radiation shielding coating, as radiowave, electromagnetic wave shielding; Can also as antistatic coating etc.
Traditional macromolecule conducting material utilizes heat curing techniques more, compare with thermofixation, photocuring technology has the advantage not available for many conventional curing technology, as high in capacity usage ratio, be suitable for that heat-sensitive substrate material, pollution-free, curing speed are fast, film good combination property and applicable continuous mass production.
Summary of the invention
The object of the invention is to design the light curable conductive coating having better performance at everyways such as weathering resistance, wear resistance, thermostability, sticking power, electroconductibility, this electrically conducting coating is widely used in the fields such as indicating meter, electrical equipment, Communication Equipment, electronic product.
Technical scheme of the present invention: a kind of preparation method of light curable conductive coating, concrete steps are:
(1) preparation of photocuring sulfonate type urethane resin: add a certain amount of isophorone diisocyanate (IPDI) in the dry there-necked flask that agitator is housed, a certain amount of polycarbonate diol (PCDL2000) and the positive fourth tin (DBTDL) of catalyst dibutyltin cinnamic acid two is added in dropping funnel, shake up, drip, be warming up to 50 DEG C; After dropwising, continue reaction 1h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, adding a certain amount of BDO (BDO), being warming up to 70 DEG C simultaneously; After reaction 1.5h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add a certain amount of N, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid sodium; After reaction 3h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add a certain amount of hydroxyethyl methylacrylate (HEMA) and continue reaction, whole reaction process is all with butylacetate hierarchy of control viscosity.When NCO reaches theoretical value, reaction terminates, and products therefrom is designated as A.
(2) preparation of photocuring intrinsically conducting resin: add a certain amount of product A in the dry there-necked flask that agitator is housed, add in dropping funnel by a certain amount of deionized water, the speed of dripping with 2 ~ 3s/ drips, rapid stirring reaction 4h.Take a certain amount of 3,4-ethene dioxythiophene (EDOT) joins in product A, mol ratio is 1:1.7 ~ 2.1, add a certain amount of oxygenant ammonium persulphate, catalyst sulfuric acid iron again, obtain mazarine emulsion after rapid stirring reaction 24h under room temperature, the drying gained resin that dewaters is product B.
(3) preparation of graphene-polypyrrole conducting nano powder: add appropriate tetrahydrofuran (THF) (THF) solvent in the dry there-necked flask that magnetic stir bar is housed, then add a certain amount of Graphene, ultrasonic disperse 1h.By there-necked flask as on magnetic stirring apparatus, a certain amount of Witco 1298 Soft Acid (DBSA) is slowly added under whipped state, add a certain amount of pyrrole monomer again, after vigorous stirring 20min, a certain amount of ammonium persulfate aqueous solution is added in dropping funnel, slowly be added drop-wise in reaction system, after dropwising, continue reaction 12h.After reaction terminates, suction filtration, dry gained are final product, are designated as C.
(4) preparation of light curable conductive coating: the product B and the product C that take metering in the dry there-necked flask that agitator is housed respectively; add appropriate light trigger phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide (819), reactive thinner, dispersion agent, flow agent etc. i.e. obtained light curable conductive coating, through UV-irradiation and curable film-forming.
Embodiment
Embodiment 1:
13.8g isophorone diisocyanate (IPDI) is added in the dry there-necked flask that agitator is housed, 31.2g polycarbonate diol (PCDL2000) and the positive fourth tin (DBTDL) of 0.025g tin dilaurate two is added in dropping funnel, shake up, drip, be warming up to 50 DEG C; After dropwising, continue reaction 1h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 2.8g1,4-butyleneglycol (BDO), is warming up to 70 DEG C simultaneously; After reaction 1.5h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 0.8g N, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid sodium; After reaction 3h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 3.98g hydroxyethyl methylacrylate (HEMA) and continue reaction, whole reaction process is all with butylacetate hierarchy of control viscosity.When NCO reaches theoretical value, reaction terminates, and products therefrom is designated as A.
In the dry there-necked flask that agitator is housed, add 10g product A, take 10g deionized water and add in dropping funnel, the speed of dripping with 2 ~ 3s/ drips, rapid stirring reaction 4h.Take 1.5g3,4-ethene dioxythiophene (EDOT) joins in product A, and mol ratio is 1:1.7 ~ 2.1, then adds 1.8g ammonium persulphate, 0.015g ferric sulfate, obtain mazarine emulsion after rapid stirring reaction 24h under room temperature, the drying gained resin that dewaters is product B.
In the dry there-necked flask that magnetic stir bar is housed, add 60mL tetrahydrofuran (THF) (THF) solvent, then add 3.5g Graphene, ultrasonic disperse 1h.By there-necked flask as on magnetic stirring apparatus, 20g Witco 1298 Soft Acid (DBSA) is slowly added under whipped state, add 10g pyrrole monomer again, after vigorous stirring 20min, the aqueous solution of 3.65g ammonium persulphate is added in dropping funnel, slowly be added drop-wise in reaction system, after dropwising, continue reaction 12h.After reaction terminates, suction filtration, dry gained are final product, are designated as C.
20g product B and 5g product C is taken respectively in the dry there-necked flask that agitator is housed; add 1.2g light trigger phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide (819), 2g reactive thinner, 0.15g dispersion agent, 0.15g flow agent etc. i.e. obtained light curable conductive coating, through UV-irradiation and curable film-forming.
Embodiment 2:
22.2g isophorone diisocyanate (IPDI) is added in the dry there-necked flask that agitator is housed, 35.3g polycarbonate diol (PCDL2000) and the positive fourth tin (DBTDL) of 0.03g tin dilaurate two is added in dropping funnel, shake up, drip, be warming up to 50 DEG C; After dropwising, continue reaction 1h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 3.4g1,4-butyleneglycol (BDO), is warming up to 70 DEG C simultaneously; After reaction 1.5h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 1.2g N, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid sodium; After reaction 3h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add 4.35g hydroxyethyl methylacrylate (HEMA) and continue reaction, whole reaction process is all with butylacetate hierarchy of control viscosity.When NCO reaches theoretical value, reaction terminates, and products therefrom is designated as A.
In the dry there-necked flask that agitator is housed, add 20g product A, take 25g deionized water and add in dropping funnel, the speed of dripping with 2 ~ 3s/ drips, rapid stirring reaction 4h.Take 2.3g3,4-ethene dioxythiophene (EDOT) joins in product A, and mol ratio is 1:1.7 ~ 2.1, then adds 2.1g ammonium persulphate, 0.023g ferric sulfate, obtain mazarine emulsion after rapid stirring reaction 24h under room temperature, the drying gained resin that dewaters is product B.
In the dry there-necked flask that magnetic stir bar is housed, add 100mL tetrahydrofuran (THF) (THF) solvent, then add 4.5g Graphene, ultrasonic disperse 1h.By there-necked flask as on magnetic stirring apparatus, 25g Witco 1298 Soft Acid (DBSA) is slowly added under whipped state, add 15g pyrrole monomer again, after vigorous stirring 20min, the aqueous solution of 4.75g ammonium persulphate is added in dropping funnel, slowly be added drop-wise in reaction system, after dropwising, continue reaction 12h.After reaction terminates, suction filtration, dry gained are final product, are designated as C.
30g product B and 6g product C is taken respectively in the dry there-necked flask that agitator is housed; add 1.3g light trigger phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide (819), 3.5g reactive thinner, 0.22g dispersion agent, 0.22g flow agent etc. i.e. obtained light curable conductive coating, through UV-irradiation and curable film-forming.
Claims (1)
1. a preparation method for light curable conductive coating, is characterized in that, comprises the steps:
(1) preparation of photocuring sulfonate type urethane resin: add a certain amount of isophorone diisocyanate (IPDI) in the dry there-necked flask that agitator is housed, a certain amount of polycarbonate diol (PCDL2000) and the positive fourth tin (DBTDL) of catalyst dibutyltin cinnamic acid two is added in dropping funnel, shake up, drip, be warming up to 50 DEG C; After dropwising, continue reaction 1h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, adding a certain amount of BDO (BDO), being warming up to 70 DEG C simultaneously; After reaction 1.5h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add a certain amount of N, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid sodium; After reaction 3h, with the change of nco value in Di-n-Butyl Amine method monitoring system, when reaching theoretical value, add a certain amount of hydroxyethyl methylacrylate (HEMA) and continue reaction, whole reaction process is all with butylacetate hierarchy of control viscosity.When NCO reaches theoretical value, reaction terminates, and products therefrom is designated as A.
(2) preparation of photocuring intrinsically conducting resin: add a certain amount of product A in the dry there-necked flask that agitator is housed, add in dropping funnel by a certain amount of deionized water, the speed of dripping with 2 ~ 3s/ drips, rapid stirring reaction 4h.Take a certain amount of 3,4-ethene dioxythiophene (EDOT) joins in product A, mol ratio is 1:1.7 ~ 2.1, add a certain amount of oxygenant ammonium persulphate, catalyst sulfuric acid iron again, obtain mazarine emulsion after rapid stirring reaction 24h under room temperature, the drying gained resin that dewaters is product B.
(3) preparation of graphene-polypyrrole conducting nano powder: add appropriate tetrahydrofuran (THF) (THF) solvent in the dry there-necked flask that magnetic stir bar is housed, then add a certain amount of Graphene, ultrasonic disperse 1h.By there-necked flask as on magnetic stirring apparatus, a certain amount of Witco 1298 Soft Acid (DBSA) is slowly added under whipped state, add a certain amount of pyrrole monomer again, after vigorous stirring 20min, a certain amount of ammonium persulfate aqueous solution is added in dropping funnel, slowly be added drop-wise in reaction system, after dropwising, continue reaction 12h.After reaction terminates, suction filtration, dry gained are final product, are designated as C.
(4) preparation of light curable conductive coating: the product B and the product C that take metering in the dry there-necked flask that agitator is housed respectively; add appropriate light trigger phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide (819), reactive thinner, dispersion agent, flow agent etc. i.e. obtained light curable conductive coating, through UV-irradiation and curable film-forming.
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| CN201310565790.3A CN104629611A (en) | 2013-11-14 | 2013-11-14 | Method for preparing light-curing conductive coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542651A (en) * | 2015-12-30 | 2016-05-04 | 中物功能材料研究院有限公司 | Polyurethane acrylate dispersion and preparation method thereof, and ultraviolet-curing conducting paint and preparation method thereof |
| CN105602434A (en) * | 2015-12-30 | 2016-05-25 | 中物功能材料研究院有限公司 | Ultraviolet curing conductive paint and preparation method thereof |
| CN106883596A (en) * | 2017-04-01 | 2017-06-23 | 广州纽楷美新材料科技有限公司 | Polythiophene/sulfonic acid aqueous polyurethane conductive material and preparation method and application |
| CN113979991A (en) * | 2021-10-25 | 2022-01-28 | 广东邦固化学科技有限公司 | UV conductive prepolymer and preparation method thereof, and transparent conductive UV curing coating and preparation method thereof |
-
2013
- 2013-11-14 CN CN201310565790.3A patent/CN104629611A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542651A (en) * | 2015-12-30 | 2016-05-04 | 中物功能材料研究院有限公司 | Polyurethane acrylate dispersion and preparation method thereof, and ultraviolet-curing conducting paint and preparation method thereof |
| CN105602434A (en) * | 2015-12-30 | 2016-05-25 | 中物功能材料研究院有限公司 | Ultraviolet curing conductive paint and preparation method thereof |
| CN105542651B (en) * | 2015-12-30 | 2018-03-23 | 砺剑防务技术集团有限公司 | Urethane acrylate dispersoid and preparation method thereof and ultraviolet light solidification electrically-conducting paint and preparation method thereof |
| CN105602434B (en) * | 2015-12-30 | 2018-04-17 | 贾学明 | Ultraviolet light cures electrically-conducting paint and preparation method thereof |
| CN106883596A (en) * | 2017-04-01 | 2017-06-23 | 广州纽楷美新材料科技有限公司 | Polythiophene/sulfonic acid aqueous polyurethane conductive material and preparation method and application |
| CN106883596B (en) * | 2017-04-01 | 2019-06-07 | 广州纽楷美新材料科技有限公司 | Polythiophene/sulfonic acid aqueous polyurethane conductive material and the preparation method and application thereof |
| CN113979991A (en) * | 2021-10-25 | 2022-01-28 | 广东邦固化学科技有限公司 | UV conductive prepolymer and preparation method thereof, and transparent conductive UV curing coating and preparation method thereof |
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Application publication date: 20150520 |