CN101624491B - Water-based driography electrically conductive ink and preparation method thereof - Google Patents

Water-based driography electrically conductive ink and preparation method thereof Download PDF

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Publication number
CN101624491B
CN101624491B CN 200810128385 CN200810128385A CN101624491B CN 101624491 B CN101624491 B CN 101624491B CN 200810128385 CN200810128385 CN 200810128385 CN 200810128385 A CN200810128385 A CN 200810128385A CN 101624491 B CN101624491 B CN 101624491B
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water
electrically conductive
tric
fraction
volume
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CN101624491A (en
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李路海
李斌
莫黎昕
李仲晓
李亚玲
罗世永
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YATUSHI PRINT CO Ltd HESHAN
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YATUSHI PRINT CO Ltd HESHAN
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Abstract

The invention relates to a water-based driography electrically conductive ink. A conductive substance of the ink adopts a conducting polymer based on poly-ethylene-dioxythiophene. The water-based driography electrically conductive ink comprises water-based polymer resin, conductive polymer aqueous dispersion solution, propanetriol, dimethyl sulfoxide, N,N-dimethylethanolamine and a water-based thickening agent. The invention also relates to a method for preparing the water-based driography electrically conductive ink, which comprises the following steps: mixing the conducting polymer aqueous dispersion solution based on the poly-ethylene-dioxythiophene with the dimethyl sulfoxide according to the proportion; and mixing the water-based polymer resin with the water-based thickening agent according to a proportion for standby; adjusting the pH of the mixture to be between 7.5 and 9.5; evenly mixing the mixture with the water-based resin; and adding the propanetriol into the mixture. The electroconductive polymer printing ink and the method have the advantages of thin thickness of an ink film, high printing precision and high printing speed, and also have the advantages of environmental protection, good electroconductive performance, high stability, good adherence, non heating solidification and the like.

Description

Water-based driography electrically conductive ink and preparation method thereof
Technical field
The present invention relates to electrically conductive ink, more particularly, relate to a kind of water-based driography electrically conductive ink and preparation method thereof.
Background technology
Mostly conventional conductive printing ink is solvent-borne type, and the pollution that the volatile organic content that in production and use, is discharged produces is come after the automobile at present, classifies city primary pollution source as.Along with scientific-technical progress and rapid development of economy, the scarcity of the resource and the energy has caused the attention of countries in the world, and joint money is energy-conservation, and the protection environment is the subject matter that chemical industry interface, the world is faced.The water-base conductive printing ink of nontoxic pollution-free environment-friendly type will replace the solvent-borne type electrically conductive ink in the near future gradually.The traditional fabrication method of electrically conductive ink is with conductive silver paste or carbon slurry, adopts the mode of silk screen printing.Contain organic solvents such as a large amount of aromatic hydrocarbons, ester class, alcohols, ketone, pure ethers in its ink composition, not only contaminate environment endanger the healthy of operator, and the screen printing mode print speed is slow, and production efficiency is low; Ink film thickness is big, cost is high; Printing precision is low, can not satisfy the requirement of current electronic product for printing precision day by day.
Summary of the invention
The technical problem that the present invention will solve is, to the above-mentioned contaminate environment of prior art, the defective that ink film thickness is big, printing precision is low, a kind of water-based driography electrically conductive ink and preparation method thereof is provided.
The technical solution adopted for the present invention to solve the technical problems is: according to an aspect of the present invention; A kind of water-based driography electrically conductive ink is provided; Its conducting material has adopted the conductive polymers based on the polyvinyl dioxy thiophene; It is that 15%~50% aqueous high molecular resin, volume(tric)fraction are that 40%~75% the conductive polymers aqueous dispersions based on the polyvinyl dioxy thiophene, volume(tric)fraction are that 1%~10% USP Kosher, volume(tric)fraction are that 2%~5% DMSO 99.8MIN., volume(tric)fraction are 0.3%~1.0% N that this electrically conductive ink contains volume(tric)fraction; N-dimethylethanolamine, volume(tric)fraction are 2%~10% water-based thickener, and the various auxiliary agents that are used to adjust the electrically conductive ink printability.
In water-based driography electrically conductive ink of the present invention, aqueous high molecular resin that contains in the printing ink and the water-based thickener that matches make the electrically conductive ink viscosity adjustable at 10~800 pools, are applicable to driography.
In water-based driography electrically conductive ink of the present invention, said printing ink is conductive filler material with the conductive polymers aqueous dispersions based on the polyvinyl dioxy thiophene.
In water-based driography electrically conductive ink of the present invention, said aqueous high molecular resin comprises: derivatived cellulose, modified oil, modified polybutadiene resin, aqueous epoxy resins, aqueous alkide resin, water-compatible amino resin, aqueous polyester resin, aqueous phenolic aldehyde resin, water-borne acrylic resin, waterborne polyurethane resin, polyvinyl alcohol resin, waterborne organic silicon resin, water-based organic fluorine.
In water-based driography electrically conductive ink of the present invention, said water-based thickener comprises: inorganic thickening agent, cellulose family, polyacrylate(s), association type polyurethane thickener.
In water-based driography electrically conductive ink of the present invention, said mineral-type thickening material comprises: wilkinite, attapulgite, pure aluminium silicate.
In water-based driography electrically conductive ink of the present invention, said cellulose thickener comprises: methylcellulose gum, CMC 99.5, Natvosol, Vltra tears.
In water-based driography electrically conductive ink of the present invention, said polyacrylate-type thickeners comprises: the homopolymer of water miscible polyacrylate, vinylformic acid, methylacrylic acid or copolymer emulsion thickening material.
According to a further aspect in the invention, provide a kind of water-based driography electrically conductive ink making method, comprise the steps:
The DMSO 99.8MIN. that (a) will account for based on the conductive polymers aqueous dispersions massfraction 2%~5% of polyvinyl dioxy thiophene mixes with it, to improve the electroconductibility of conductive polymers;
(b) mix for use with water-based thickener in varing proportions by the requirement of electrically conductive ink viscosity the aqueous high molecular resin;
(c) will use N based on the conductive polymers aqueous dispersions of polyvinyl dioxy thiophene and the mixture of DMSO 99.8MIN., it is 7.5~9.5 that the N-dimethylethanolamine transfers to pH;
(d) be that 7.5~9.5 (c) middle mixture and the water-base resin that passes through the water-based thickener thickening mix with pH;
(e) in mixture described in the step (d), adding volume(tric)fraction is 1%~10% USP Kosher, and the auxiliary agent that is used to adjust the electrically conductive ink printability, is uniformly dispersed and promptly makes required electrically conductive ink.
In the making method of water-based driography electrically conductive ink of the present invention, said water-based thickener comprises inorganic thickening agent, cellulose family, polyacrylate(s), association type polyurethane thickener.
In the making method of electroconductive polymer printing ink of the present invention, said inorganic thickening agent comprises wilkinite, attapulgite, pure aluminium silicate.
In the making method of water-based driography electrically conductive ink of the present invention, said cellulose thickener comprises: methylcellulose gum, CMC 99.5, Natvosol, Vltra tears.
In the making method of water-based driography electrically conductive ink of the present invention, said polyacrylate-type thickeners comprises: the homopolymer of water miscible polyacrylate, vinylformic acid, methylacrylic acid or copolymer emulsion thickening material.
In the making method of water-based driography electrically conductive ink of the present invention, said aqueous high molecular resin comprises: derivatived cellulose, modified oil, modified polybutadiene resin, aqueous epoxy resins, aqueous alkide resin, water-compatible amino resin, aqueous polyester resin, aqueous phenolic aldehyde resin, water-borne acrylic resin, waterborne polyurethane resin, polyvinyl alcohol resin, waterborne organic silicon resin, water-based organic fluorine.
Water-based driography electrically conductive ink of embodiment of the present invention and preparation method thereof; Have following beneficial effect: the invention provides a kind of water-soluble conducting ink that is applicable to offset printing, gravure and silk-screen, its conductive filler material is based on the conductive polymers aqueous dispersions of polyvinyl dioxy thiophene.Adopt aqueous high molecular and water-based thickener to be used as the conductive oil ink connecting material; With other auxiliary agent that is used to adjust printing ink conductivity and printability electrically conductive ink that processes from strand; This printing ink is because can adopt the mode of driography to print; Have that ink film thin thickness, printing precision are high, the fast characteristics of print speed, characteristics such as having environmental protection simultaneously, conduct electricity very well, stability is high, sticking power is good, need not to be heating and curing.The silk-screen product need not be heating and curing yet, as long as warm air drying promptly possesses good water tolerance.
Description of drawings
To combine accompanying drawing and embodiment that the present invention is described further below, in the accompanying drawing:
Fig. 1 is that the viscosity of water-based driography electrically conductive ink of the first embodiment of the present invention is with change in rotational speed rule synoptic diagram;
Fig. 2 is that the viscosity of water-based driography electrically conductive ink of the second embodiment of the present invention is with change in rotational speed rule synoptic diagram;
Fig. 3 is that the viscosity of water-based driography electrically conductive ink of the third embodiment of the present invention is with change in rotational speed rule synoptic diagram.
Embodiment
Through instance the present invention is further illustrated below, instance only is the present invention is described and never limits the present invention.
First embodiment: take by weighing 60.0% conductive polymers aqueous dispersions by prescription, the DMSO 99.8MIN. that accounts for based on the conductive polymers aqueous dispersions 5.0% of polyvinyl dioxy thiophene is mixed with it to improve electroconductibility based on the polyvinyl dioxy thiophene; Take by weighing 30.0% waterborne polyurethane resin, and add the water-based thickener that accounts for waterborne polyurethane resin 4% and mix with it, and grind 10min with uniform mixing with three-roll grinder; The N of adding 0.8%, the pH of mixed that the N-dimethylethanolamine is regulated conductive polymers and DMSO 99.8MIN. is 8.5~9, subsequently its waterborne polyurethane resin with the process thickening is mixed; Add ink addition agents such as 5.0% USP Kosher and a certain amount of skimmer, flow agent again, promptly make required electrically conductive ink (above per-cent is volume(tric)fraction) behind the homodisperse.Above-mentioned water-based thickener comprises any in inorganic thickening agent, cellulose family, polyacrylate(s), the association type polyurethane thickener or two or more combination; Above-mentioned inorganic thickening agent comprises: wilkinite, attapulgite, pure aluminium silicate; Above-mentioned cellulose thickener comprises: methylcellulose gum, CMC 99.5, Natvosol, Vltra tears; Above-mentioned polyacrylate-type thickeners comprises: the homopolymer of water miscible polyacrylate, vinylformic acid, methylacrylic acid or copolymer emulsion thickening material.
The Specifeca tion speeification of the electrically conductive ink product of preparation is as shown in table 1 below according to the above ratio:
The electrically conductive ink performance perameter of table 1 first embodiment
Project Performance perameter Examination criteria
Viscosity (P) 644~181 BROOKFIELD DV-II+Pro VISCOMTER
Stickiness 2.4 YQM-1B ink viscosity appearance
The pH value 8.5~9
Surface tension (mN/m) 44.079 Germany KRUSS K100
Surface resistivity (k Ω/cm 2) About 80~1600 is adjustable according to thickness
Ink film thickness (μ m) About 0.8~3 is adjustable according to printing condition
Sticking power
100/100 GB/T12347.7-1991
Thermotolerance (25 ± 1 ℃, 24h) 17%
" BROOKFIELD DV-II+Pro VISCOMTER " in the table is meant the viscosity of the BROOKFIELD viscosmeter mensuration printing ink of producing with U.S. BROOKFIELD company, and model is the DV-II+Pro type." YQM-1B ink viscosity appearance " is meant and adopts YQM-1B type ink viscosity appearance that the stickiness of printing ink is measured." German KRUSS K100 " is meant the surface tension of the surface tension instrument K100 mensuration printing ink that the German KRUSS of employing company produces." GB/T12347.7-1991 " is meant that employing standard GB/T12347.7-1991 measures the sticking power of printing ink (hereinafter this no longer being carried out repeat specification).
Electrically conductive ink according to the foregoing description preparation has the rheological of shear shinning, and its viscosity is as shown in Figure 1 with the change curve of shearing rate.This is because under high shear rate, the associative structure of resin structure and water-based thickener and resin is destroyed and causes viscosity to reduce, when shearing force disappearance viscosity can recover again.Transfer on ink roller is favourable for printing ink in the printing process for this.
Second embodiment: take by weighing 71.7% conductive polymers aqueous dispersions by prescription, the DMSO 99.8MIN. that accounts for based on the conductive polymers aqueous dispersions 5.0% of polyvinyl dioxy thiophene is mixed with it to improve electroconductibility based on the polyvinyl dioxy thiophene; Take by weighing 17.9% waterborne polyurethane resin, and add the water-based thickener that accounts for waterborne polyurethane resin 8% and mix with it, and grind 10min with uniform mixing with three-roll grinder; 0.8% N, the pH of mixed that the N-dimethylethanolamine is regulated conductive polymers and DMSO 99.8MIN. is 8.5~9, subsequently its waterborne polyurethane resin with the process thickening is mixed; Add ink addition agents such as 5.0% USP Kosher and a certain amount of skimmer, flow agent again, promptly make required electrically conductive ink (above per-cent is volume(tric)fraction) behind the homodisperse.Above-mentioned water-based thickener comprises any in inorganic thickening agent, cellulose family, polyacrylate(s), the association type polyurethane thickener or two or more combination; Above-mentioned inorganic thickening agent comprises: wilkinite, attapulgite, pure aluminium silicate; Above-mentioned cellulose thickener comprises: methylcellulose gum, CMC 99.5, Natvosol, Vltra tears; Above-mentioned polyacrylate-type thickeners comprises: the homopolymer of water miscible polyacrylate, vinylformic acid, methylacrylic acid or copolymer emulsion thickening material.
The Specifeca tion speeification of the electrically conductive ink product of preparation is as shown in table 2 below according to the above ratio:
The electrically conductive ink performance perameter of table 2 second embodiment
Project Performance perameter Examination criteria
Viscosity (P/25 ℃) 92~14 BROOKFIELD DV-II+Pro VISCOMTER
Stickiness 2.4 YQM-1B ink viscosity appearance
The pH value 8.5~9
Surface tension (mN/m) 39.660 Germany KRUSS K100
Surface resistivity (k Ω/cm 2) About 80~1600 is adjustable according to thickness
Ink film thickness (μ m) About 0.8~3 is adjustable
Sticking power
100/100 GB/T12347.7-1991
Thermotolerance (25 ± 1 ℃, 24h) 17%
Electrically conductive ink according to the foregoing description preparation has the rheological of shear shinning, and its viscosity is as shown in Figure 2 with the change curve of shearing rate.This is because under high shear rate, the associative structure of resin structure and water-based thickener and resin is destroyed and causes viscosity to reduce, when shearing force disappearance viscosity can recover again.Transfer on ink roller is favourable for printing ink in the printing process for this.
The 3rd embodiment: take by weighing 66.6% conductive polymers aqueous dispersions by prescription, the DMSO 99.8MIN. that accounts for based on the conductive polymers aqueous dispersions 5.0% of polyvinyl dioxy thiophene is mixed with it to improve electroconductibility based on the polyvinyl dioxy thiophene; Take by weighing 22.2% waterborne polyurethane resin, and add the water-based thickener that accounts for waterborne polyurethane resin 8% and mix with it, and grind 10min with uniform mixing with three-roll grinder; 0.8% N, the pH of mixed that the N-dimethylethanolamine is regulated conductive polymers and DMSO 99.8MIN. is 8.5~9, subsequently its waterborne polyurethane resin with the process thickening is mixed; Add ink addition agents such as 5.0% USP Kosher and a certain amount of skimmer, flow agent again, promptly make required electrically conductive ink (above per-cent is volume(tric)fraction) behind the homodisperse.Above-mentioned water-based thickener comprises any in inorganic thickening agent, cellulose family, polyacrylate(s), the association type polyurethane thickener or two or more combination; Above-mentioned inorganic thickening agent comprises: wilkinite, attapulgite, pure aluminium silicate; Above-mentioned cellulose thickener comprises: methylcellulose gum, CMC 99.5, Natvosol, Vltra tears; Above-mentioned polyacrylate-type thickeners comprises: the homopolymer of water miscible polyacrylate, vinylformic acid, methylacrylic acid or copolymer emulsion thickening material.
The electrically conductive ink performance perameter of table 3 the 3rd embodiment
Project Performance perameter Examination criteria
Viscosity (P/25 ℃) 659~124 BROOKFIELD DV-II+Pro?VISCOMTER
Stickiness 2.0 YQM-1B ink viscosity appearance
The pH value 8.5~9
Surface tension (mN/m) 42.746 Germany KRUSS K100
Surface resistivity (k Ω/cm 2) About 80~1600 is adjustable according to thickness
Ink film thickness (μ m) About 0.8~3 is adjustable
Sticking power
100/100 GB/T12347.7-1991
Thermotolerance (25 ± 1 ℃, 24h) 17%
Electrically conductive ink according to the foregoing description preparation has the rheological of shear shinning, and its viscosity is as shown in Figure 3 with the change curve of shearing rate.This is because under high shear rate, the associative structure of resin structure and water-based thickener and resin is destroyed and causes viscosity to reduce, when shearing force disappearance viscosity can recover again.Transfer on ink roller is favourable for printing ink in the printing process for this.
In above-mentioned first, second, third embodiment of the present invention, waterborne polyurethane resin is also replaceable to be other aqueous high molecular resins such as derivatived cellulose, modified oil, modified polybutadiene resin, aqueous epoxy resins, aqueous alkide resin, water-compatible amino resin, aqueous polyester resin, aqueous phenolic aldehyde resin, water-borne acrylic resin, waterborne polyurethane resin, polyvinyl alcohol resin, waterborne organic silicon resin, water-based organic fluorine of same content.

Claims (2)

1. the making method of a water-based driography electrically conductive ink is characterized in that, comprises the steps:
(a) taking by weighing volume(tric)fraction is 66.6% the conductive polymers aqueous dispersions based on the polyvinyl dioxy thiophene, is that 3.33% DMSO 99.8MIN. mixes with it with volume(tric)fraction, to improve the electroconductibility of conductive polymers;
(b) taking by weighing volume(tric)fraction is 22.2% waterborne polyurethane resin, is that 1.776% water-based thickener mixes for use with volume(tric)fraction;
(c) will use volume(tric)fraction based on the mixture of the conductive polymers aqueous dispersions of polyvinyl dioxy thiophene and DMSO 99.8MIN. is 0.8% N, and it is 8.5~9 that the N-dimethylethanolamine transfers to pH;
(d) be that 8.5~9 (c) middle mixture and the waterborne polyurethane resin that passes through the water-based thickener thickening mix with pH;
(e) in mixture described in the step (d), adding volume(tric)fraction is 5% USP Kosher, and the auxiliary agent that is used to adjust the electrically conductive ink printability, is uniformly dispersed and promptly makes required electrically conductive ink.
2. water-based driography electrically conductive ink of making according to the method for claim 1; It is characterized in that; Its conducting material has adopted the conductive polymers based on the polyvinyl dioxy thiophene; It is that 22.2% waterborne polyurethane resin, volume(tric)fraction are that 66.6% the conductive polymers aqueous dispersions based on the polyvinyl dioxy thiophene, volume(tric)fraction are that 5.0% USP Kosher, volume(tric)fraction are that 3.33% DMSO 99.8MIN., volume(tric)fraction are 0.8% N that this electrically conductive ink contains volume(tric)fraction; N-dimethylethanolamine, volume(tric)fraction are 1.776% water-based thickener, and the various auxiliary agents that are used to adjust the electrically conductive ink printability.
CN 200810128385 2008-07-07 2008-07-07 Water-based driography electrically conductive ink and preparation method thereof Expired - Fee Related CN101624491B (en)

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CN 200810128385 CN101624491B (en) 2008-07-07 2008-07-07 Water-based driography electrically conductive ink and preparation method thereof
HK10106174.3A HK1140224A1 (en) 2008-07-07 2010-06-23 Water-based waterless offset and electrically conductive printing ink and method of production thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102311683A (en) * 2011-09-23 2012-01-11 传美讯电子科技(珠海)有限公司 Ink-jet printing pigment ink used on coating-free medium
CN108148471A (en) * 2016-12-05 2018-06-12 洛阳尖端技术研究院 A kind of electrically conductive ink and preparation method thereof
CN110982338A (en) * 2019-12-20 2020-04-10 江苏正红彩印有限公司 Aqueous thermosetting printing ink
CN113436805A (en) * 2021-04-29 2021-09-24 哈工大机器人集团(无锡)科创基地研究院 Preparation method and application of low-silver aqueous conductive silver paste

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1439029A (en) * 2000-06-26 2003-08-27 爱克发-格法特公司 Redispersible latex comprising a polythiophene
CN1527854A (en) * 2001-03-29 2004-09-08 ����-�����ع�˾ Aqueous composition containing polymer or copolymer of a 3,4-dialkoxythiophene and a non-Newtonian binder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1439029A (en) * 2000-06-26 2003-08-27 爱克发-格法特公司 Redispersible latex comprising a polythiophene
CN1527854A (en) * 2001-03-29 2004-09-08 ����-�����ع�˾ Aqueous composition containing polymer or copolymer of a 3,4-dialkoxythiophene and a non-Newtonian binder

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HK1140224A1 (en) 2010-10-08

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