CN103865464B - Water-based conductive adhesive and preparation method thereof - Google Patents
Water-based conductive adhesive and preparation method thereof Download PDFInfo
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- CN103865464B CN103865464B CN201410106754.5A CN201410106754A CN103865464B CN 103865464 B CN103865464 B CN 103865464B CN 201410106754 A CN201410106754 A CN 201410106754A CN 103865464 B CN103865464 B CN 103865464B
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Abstract
The invention provides a water-based conductive adhesive and a preparation method of the adhesive, which belong to the technical field of adhesives and aim at solving the problem of poor adhesion performance of the existing conductive adhesive. The water-based conductive adhesive contains the following components in parts by mass: 48-75 parts of water-based polyurethane emulsion, 3-7 parts of poly-3,4-ethylenedioxythiophene-polystyrolsulfon acid, 1-5 parts of talcum powder, 3-8 parts of a coupling agent, 2.4-5.2 parts of a water-based curing agent, 0.15-0.42 part of a leveling agent, 5-12 parts of a water-based film-forming additive and 0.08-0.17 part of organic bentonite. The invention also provides the preparation method of the water-based conductive adhesive. The water-based conductive adhesive does not contain any volatile 'tribenzyl' substance and consequently does not cause any pollution to environment, and the stripping resistance of the water-based conductive adhesive can achieve 110N/cm.
Description
Technical field
The invention belongs to technical field of adhesive, be specifically related to a kind of waterborne conductive tackiness agent and preparation method thereof.
Background technology
Electro-conductive adhesive is a kind of tackiness agent solidifying or have certain conductivity after drying, usual preparation method is for filmogen with matrix resin and solidifying agent, conductive filler material is conductive additive, by the bonding effect of matrix resin, conducting particles is combined together to form conductive network passage, realizes being connected by the conduction of adhesives.Electro-conductive adhesive chief component is matrix resin, solidifying agent, conductive additive and auxiliary agent composition.Up to the present, conductive filler material adopts the inorganic materials such as conductive carbon black, electrically conductive graphite, Graphene and metal powder to be conductive additive mostly.Patent 201110246296.1 reports a kind of preparation method of electro-conductive adhesive, take epoxy resin as filmogen, and hexanediamine and thanomin are solidifying agent, and dioctyl phthalate (DOP) is softening agent, and copper powder is that conductive additive has prepared electro-conductive adhesive.Patent 201010572271.6 reports a kind of epoxy resin conductive adhesive and preparation method thereof, and with the flake silver powder of graphene modified for conductive additive, epoxy resin and solidifying agent are filmogen, have prepared electro-conductive adhesive.But these conductive additives are mineral-type materials, be difficult to be evenly dispersed in adhesive system, greatly reduce the cementability of tackiness agent.Conducting polymer composite, as conductive additive, can have good consistency with the matrix resin of tackiness agent, can not have any impact to the cementability of tackiness agent, is the one effective means the most replacing inorganic conductive filler to prepare electro-conductive adhesive.Along with the development trend of global green material, environment-friendly water-based conductive tackiness agent becomes the developing direction of adhesive area.Patent 201210256663.0 reports a kind of waterborne conductive glue for lithium ion battery, its technological core take graphite as conductive additive, acrylic copolymer is film-forming resin, and Virahol is aqueous promoter, adds KH-560 simultaneously and has prepared waterborne conductive glue as coupling agent.But this aqueous adhesive is still using inorganic materials graphite as conductive additive, certain impact can be brought on adhesiveproperties.
Summary of the invention
The object of the invention is the problem in order to solve existing electro-conductive adhesive bad adhesion, and a kind of environmental-friendly aqueous electro-conductive adhesive and preparation method thereof is provided.
First the present invention provides a kind of waterborne conductive tackiness agent, according to mass fraction meter, comprising:
Preferably, it is one in Sancure12954, Sancure2026, Sancure815, Sancure825, Sancure835, Sancure843 or Sancure898 that described aqueous polyurethane emulsion is selected from the model that German Lubrizol Corp. produces.
Preferably, the specific conductivity of described poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid is 1.0 × 10
4-1.0 × 10
5ohm/m
2.
Preferably, described talcum powder is 800-1280 object talcum powder.
Preferably, described coupling agent is the one in KH-550, KH560, KH-570 or KH-792.
Preferably, described waterborne curing agent be selected from Bayhydur3100, BayhydurXP2547, DesmodurD or BayhydurXP2451 any one or a few.
Preferably, described water-based flow agent is selected from one or more in BYK-380, BYK-307, BYK-341, BYK-381 or BYK-345.
Preferably, described waterborne film-forming auxiliary agent is selected from one or more in butyl glycol ether, butyl, Virahol, propyl carbinol or propylene glycol.
Preferably, described organobentonite is this Bentone38 organobentonite of hamming.
The present invention also provides a kind of preparation method of waterborne conductive tackiness agent, comprises the following steps:
According to mass fraction meter, by aqueous polyurethane emulsion, poly-3,4-ethene dioxythiophene-polystyrolsulfon acid, talcum powder, coupling agent, water-based flow agent and organobentonite mix, sand milling 1.5 ~ 3 hours after stirring, add waterborne curing agent and waterborne film-forming auxiliary agent again, agitation and filtration, obtains waterborne conductive tackiness agent.
Beneficial effect of the present invention:
First the present invention provides a kind of electro-conductive adhesive, this electro-conductive adhesive is with poly-3,4-ethene dioxythiophene-polystyrolsulfon acid (PEDOT-PSS) water-based conducting polymer is the waterborne conductive tackiness agent of conductive additive, this conductive additive can have good consistency with the matrix water-base resin in waterborne conductive adhesive system of the present invention as aqueous high molecular, thus, form a kind of aqueous adhesive of homogeneous phase, make the waterborne conductive glue obtained have excellent bonding force; Simultaneously, compared with traditional solvent-borne type electro-conductive adhesive, not containing any poisonous and harmful " triphen " class volatile matter in aqueous adhesive of the present invention, can not cause any pollution to environment, experimental result shows: electro-conductive adhesive peeling force of the present invention can reach 110N/cm.
The present invention also provides a kind of preparation method of electro-conductive adhesive, the method is with poly-3,4-ethene dioxythiophene-polystyrolsulfon acid (PEDOT-PSS) water-based conducting polymer is conductive additive, using aqueous polyurethane as filmogen, water-based polyisocyanates, as waterborne curing agent, has prepared waterborne conductive tackiness agent.This preparation method is simple, obtains electro-conductive adhesive and has excellent adhesiveproperties.
Embodiment
First the present invention provides a kind of waterborne conductive tackiness agent, according to mass fraction meter, comprising:
Aqueous polyurethane emulsion 48-75 part, poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid 3-7 part, talcum powder 1-5 part, coupling agent 3-8 part, waterborne curing agent 2.4-5.2 part, water-based flow agent 0.15-0.42 part, waterborne film-forming auxiliary agent 5-12 part, organobentonite 0.08-0.17 part; Be preferably aqueous polyurethane emulsion 50-70 part, poly-3,4-ethene dioxythiophene-polystyrolsulfon acid 4.5-6.5 part, talcum powder 2.6-4.5 part, coupling agent 4.8-7.5 part, waterborne curing agent 3.5-5.0 part, water-based flow agent 0.22-0.40 part, waterborne film-forming auxiliary agent 7-10.5 part, organobentonite 0.10-0.15 part.
According to the present invention, described aqueous polyurethane emulsion is preferably selected from the one in Sancure12954, Sancure2026, Sancure815, Sancure825, Sancure835, Sancure843 or Sancure898 of German Lu Borun.The present invention adopts aqueous polyurethane as film-forming resin, and can improve the sticking power with base material, polyurethane system and PEDOT-PSS have again good consistency, can improve the cohesiveness of waterborne conductive tackiness agent.
According to the present invention, the specific conductivity of described poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid (PEDOT-PSS) is preferably 1.0 × 10
4-1.0 × 10
5ohm/m
2.The number-average molecular weight of described poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid is preferably 8000-14000 dalton, and solid content is preferably 1-1.4%.The present invention uses poly-3,4-ethene dioxythiophene-polystyrolsulfon acid (PEDOT-PSS) water-based conducting polymer is as conductive additive, this conductive additive can have good consistency with the matrix water-base resin in waterborne conductive adhesive system as aqueous high molecular, thus, form a kind of aqueous adhesive of homogeneous phase, make the waterborne conductive glue obtained have excellent bonding force.
According to the present invention, described talcum powder is preferably 800-1280 object talcum powder.
According to the present invention, described coupling agent is silane coupling agent, and preferably model is the one in KH-550, KH560, KH-570 or KH-792.
According to the present invention, described waterborne curing agent is water dispersible polyisocyanate, and being preferably the model that Bayhydur company produces is any one or a few in Bayhydur3100, BayhydurXP2547, DesmodurD or BayhydurXP2451.
According to the present invention, it is one or more in BYK-380, BYK-307, BYK-341, BYK-381 or BYK-345 that described water-based flow agent is preferably the model that BYK company produces.
According to the present invention, described waterborne film-forming auxiliary agent is preferably selected from one or more in butyl glycol ether, butyl, Virahol, propyl carbinol or propylene glycol.The effect of waterborne film-forming auxiliary agent is the waterborne conductive tackiness agent more stable homogeneous making to obtain.
According to the present invention, described organobentonite is preferably this Bentone38 organobentonite of hamming.
The present invention also provides a kind of preparation method of waterborne conductive tackiness agent, comprises the following steps:
According to mass fraction meter, by aqueous polyurethane emulsion, poly-3,4-ethene dioxythiophene-polystyrolsulfon acid, talcum powder, coupling agent, water-based flow agent and organobentonite mix, sand milling 1.5 ~ 3 hours after stirring, described stirring velocity is preferably 1500 ~ 3000rpm, be more preferably 2000rpm, add waterborne curing agent and waterborne film-forming auxiliary agent again, agitation and filtration, described stirring velocity is preferably 1800 ~ 3000rpm, be more preferably 2600rpm, churning time is preferably 20-35min, obtains waterborne conductive tackiness agent.
By the waterborne conductive tackiness agent obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force.By conductive glue on a glass, dry 10min, carry out electric conductance determination for 80 DEG C.
In order to further illustrate the present invention, below in conjunction with embodiment, water-based polyurethane adhesive provided by the invention and preparation method thereof is described in detail.
Raw material involved in embodiment is commercially available.
Embodiment 1
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure12954,3g of 48g, (specific conductivity is 1.0 × 10
4ohm/m
2molecular weight is 8000 dalton), this Bentone38 organobentonite of hamming mixing of water-based flow agent BYK-380 and 0.08g of the talcum powder (1280 order) of 1g, coupling agent KH-550,0.15g of 3g, sand milling 1.5 hours after stirring, described stirring velocity is 2000rpm;
Under agitation, add the waterborne film-forming auxiliary agent butyl glycol ether of waterborne curing agent Bayhydur3100,5g of 2.4g, height filters after stirring 20min, and described stirring velocity is 2500rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 1 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 85N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 5 × 10 for 80 DEG C
5ohm/m
2.
Embodiment 2
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure2026,7g of 75g, (specific conductivity is 1.0 × 10
5ohm/m
2molecular weight is 14000 dalton), this Bentone38 organobentonite of hamming mixing of water-based flow agent BYK-307 and 0.17g of the talcum powder (1280 order) of 5g, coupling agent KH560,0.42g of 8g, sand milling 3 hours after stirring, described stirring velocity is 1800rpm;
Under agitation, add the waterborne film-forming auxiliary agent butyl of waterborne curing agent BayhydurXP2547,12g of 5.2g, height filters after stirring 35min, and described stirring velocity is 2600rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 2 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 102N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 7.5 × 10 for 80 DEG C
5ohm/m
2.
Embodiment 3
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure815,5g of 52g, (specific conductivity is 1.0 × 10
5ohm/m
2molecular weight is 10000 dalton), this Bentone38 organobentonite of hamming mixing of water-based flow agent BYK-381 and 0.12g of the talcum powder (1280 order) of 2.6g, coupling agent KH-550,0.22g of 4.8g, sand milling 2 hours after stirring, described stirring velocity is 3000rpm;
Under agitation, add the waterborne film-forming auxiliary agent propylene glycol of waterborne curing agent DesmodurD, 7g of 3.5g, height filters after stirring 30min, and described stirring velocity is 3000rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 3 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 92N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 8.5 × 10 for 80 DEG C
5ohm/m
2.
Embodiment 4
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure835,5.8g of 63g, (specific conductivity is 1.0 × 10
5ohm/m
2molecular weight is 12000 dalton), this Bentone38 organobentonite of hamming mixing of water-based flow agent BYK-341 and 0.10g of the talcum powder (800 order) of 3.5g, coupling agent KH-792,0.31g of 5g, sand milling 2.5 hours after stirring, described stirring velocity is 2000rpm;
Under agitation, add the waterborne film-forming auxiliary agent diethylene glycol ether of waterborne curing agent BayhydurXP2451,8g of 4.0g, height filters after stirring 25min, and described stirring velocity is 1800rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 4 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 110N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 1.4 × 10 for 80 DEG C
4ohm/m
2.
Embodiment 5
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure825,4.5g of 50g, (specific conductivity is 1.0 × 10
4ohm/m
2molecular weight is 9000 dalton), this Bentone38 organobentonite of hamming mixing of the talcum powder (900 order) of 3.2g, the coupling agent kh-570 of 5.4g, water-based flow agent BYK-345 and 0.15g of 0.28g, sand milling 2 hours after stirring, described stirring velocity is 2200rpm;
Under agitation, add the waterborne film-forming auxiliary agent Virahol of waterborne curing agent BayhydurXP2547,8.5g of 4.7g, height filters after stirring 35min, and described stirring velocity is 2600rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 5 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 68N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 2.7 × 10 for 80 DEG C
4ohm/m
2.
Embodiment 6
By the poly-3,4-rthylene dioxythiophene-polystyrolsulfon acid of aqueous polyurethane emulsion Sancure843,6.5g of 70g, (specific conductivity is 1.0 × 10
4ohm/m
2molecular weight is 10000 dalton), this Bentone38 organobentonite of hamming mixing of water-based flow agent BYK-307 and 0.14g of the talcum powder (1280 order) of 4.5g, coupling agent KH-560,0.40g of 7.5g, sand milling 2.5 hours after stirring, described stirring velocity is 2500rpm;
Under agitation, add the waterborne film-forming auxiliary agent propyl carbinol of waterborne curing agent Bayhydur3100,10.5g of 5g, height filters after stirring 30min, and described stirring velocity is 2500rpm, obtains waterborne conductive tackiness agent.
Waterborne conductive tackiness agent embodiment 6 obtained, be sprayed on ABS plastic base material and PET non-woven fabrics, quantity for spray is 160g/m
2, dry 2min at 80 DEG C, then carry out bonding, carry out peel test force, peeling force 109N/cm; By conductive glue on a glass, dry 10min, carry out electric conductance determination, specific conductivity 1.8 × 10 for 80 DEG C
5ohm/m
2.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (6)
1. a waterborne conductive tackiness agent, is characterized in that, according to mass fraction meter, comprising:
It is one in Sancure12954, Sancure2026, Sancure815, Sancure825, Sancure835, Sancure843 or Sancure898 that described aqueous polyurethane emulsion is selected from the model that German Lubrizol Corp. produces;
Described talcum powder is 800-1280 object talcum powder;
Described waterborne curing agent be selected from Bayhydur 3100, Bayhydur XP 2547, Desmodur D or BayhydurXP 2451 any one or a few.
2. a kind of waterborne conductive tackiness agent according to claim 1, is characterized in that, described coupling agent is the one in KH-550, KH560, KH-570 or KH-792.
3. a kind of waterborne conductive tackiness agent according to claim 1, is characterized in that, described water-based flow agent is selected from one or more in BYK-380, BYK-307, BYK-341, BYK-381 or BYK-345.
4. a kind of waterborne conductive tackiness agent according to claim 1, is characterized in that, described waterborne film-forming auxiliary agent is selected from one or more in butyl glycol ether, butyl, Virahol, propyl carbinol or propylene glycol.
5. a kind of waterborne conductive tackiness agent according to claim 1, is characterized in that, described organobentonite is this Bentone 38 organobentonite of hamming.
6., according to the preparation method of a kind of waterborne conductive tackiness agent of claim 1-5 described in any one, comprise the following steps:
According to mass fraction meter, by aqueous polyurethane emulsion, poly-3,4-ethene dioxythiophene-polystyrolsulfon acid, talcum powder, coupling agent, water-based flow agent and organobentonite mix, sand milling 1.5 ~ 3 hours after stirring, add waterborne curing agent and waterborne film-forming auxiliary agent again, agitation and filtration, obtains waterborne conductive tackiness agent.
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| CN103865464B true CN103865464B (en) | 2015-06-24 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104371564A (en) * | 2014-10-30 | 2015-02-25 | 田琳琳 | Conductive adhesive |
| CN113789145A (en) * | 2021-09-28 | 2021-12-14 | 上海腾烁电子材料有限公司 | LCM single-component room-temperature quick-drying conductive adhesive and preparation method thereof |
| CN115521702B (en) * | 2022-09-23 | 2023-10-17 | 湖南纳昇电子科技有限公司 | PEDOT (polyether urethane) PSS (polyphenylene sulfide) electronic coating capable of enhancing reflection and high in hardness as well as preparation method and application thereof |
Citations (3)
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| CN102002314A (en) * | 2010-09-29 | 2011-04-06 | 中国科学院长春应用化学研究所 | Nano dispersed water-based conductive primer for vehicle bumper and preparation method thereof |
| CN102253502A (en) * | 2011-04-18 | 2011-11-23 | 广州奥翼电子科技有限公司 | Bonding agent and electro-optic assembly and electrophoretic medium thereof |
| CN102399416A (en) * | 2011-07-29 | 2012-04-04 | 常州大学 | Polyether poly(3,4-ethylenedioxythiophene) (PEDOT) water dispersion and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002314A (en) * | 2010-09-29 | 2011-04-06 | 中国科学院长春应用化学研究所 | Nano dispersed water-based conductive primer for vehicle bumper and preparation method thereof |
| CN102253502A (en) * | 2011-04-18 | 2011-11-23 | 广州奥翼电子科技有限公司 | Bonding agent and electro-optic assembly and electrophoretic medium thereof |
| CN102399416A (en) * | 2011-07-29 | 2012-04-04 | 常州大学 | Polyether poly(3,4-ethylenedioxythiophene) (PEDOT) water dispersion and preparation method thereof |
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