CN103102742B - Preparation method of nano graphite conductive ink - Google Patents
Preparation method of nano graphite conductive ink Download PDFInfo
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- CN103102742B CN103102742B CN201210536362.3A CN201210536362A CN103102742B CN 103102742 B CN103102742 B CN 103102742B CN 201210536362 A CN201210536362 A CN 201210536362A CN 103102742 B CN103102742 B CN 103102742B
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Abstract
The invention discloses a preparation method of the nano graphite conductive ink. The preparation method comprises the following steps of: 1) reacting polyethylene glycol with 2,4-toluene diisocyanate to obtain isocyanate-terminated polyurethane prepolymer; 2) reacting epoxy resin with ethylene glycol monoethyl ether acetate and the isocyanate-terminated polyurethane prepolymer to obtain polyurethane modified epoxy resin; 3) adding graphite, propylene glycol methyl ether propionate, tributyl phosphate, proprylene glycol monomethyl ether, polydimethylsiloxane, methyl acryloyl oxygen group silane and dyes into a solution of polyurethane modified epoxy resin in acetone, uniformly mixing, and conducting ultrasonic shaking to obtain the nano graphite conductive ink. Through adding the nano graphite, the nano graphite conductive ink disclosed by the invention has the advantage of good electrical conductivity, low viscidity, low fragility, high elasticity and good impact resistance.
Description
Technical field
The invention belongs to technical field of ink, be specifically related to a kind of preparation method of nano-graphite electrically conductive ink.
Background technology
Flexible circuit is to realize electronics and IT products multifunction, integrated, miniaturization and key part cheaply.Along with electronic product and equipment are to future developments such as light, thin, little, low cost, multi-functional, high reliability, the consumption of flexible circuit is increasing, utilize electrically conductive ink or conductive ink by the mode of printing or printing, on flexible insulation substrate, form conducting wire and caused scientific research personnel's extensive concern.Electrically conductive ink can be divided into structure-type and filled-type two classes by its structure difference.The electrically conductive ink that is applied at present electron trade is mainly compound-type conducting ink, conductive filler material used is generally mineral filler, as gold and silver, copper, nickel, carbon black, graphite, carbon fiber etc., and low-melting ink vehicle resin is selected resol, epoxy resin, urethane etc. conventionally.Wherein epoxy resin is because of excellent property and raw material widely application in conductive polymers cheap and easy to get, but also has the shortcomings such as electroconductibility is weak, viscosity is large, fragility is large, elasticity is little, poor impact resistance, so be necessary it modified toughened.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that the nano-graphite electrically conductive ink that a kind of electroconductibility is strong, viscosity is little, fragility is little, elasticity is large, shock-resistance is good is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of nano-graphite electrically conductive ink, the steps include:
1) by polyoxyethylene glycol, heating vacuumizes dewaters to water-content≤0.2%, inflated with nitrogen protection after being cooled to 20 ~ 25 DEG C, in regulating, 80 ~ 85 DEG C of temperature, add 2,4 toluene diisocyanate, stirring reaction to-NCO content is≤4%, stopped reaction, is cooled to 20 ~ 25 DEG C, obtains isocyanate terminated base polyurethane prepolymer for use as;
2) in reaction, add epoxy resin, then add ethylene glycol ether acetate to dissolve completely, 75 ~ 80 DEG C of temperature in keeping, the more isocyanate terminated base polyurethane prepolymer for use as that adds step 1) to arrive, reaction 2.5 ~ 3h, obtains polyurethane modified epoxy resin;
3) by step 2) polyurethane modified epoxy resin of gained is dissolved in acetone, adding particle diameter is the graphite of 7～8nm, add again propylene glycol monomethyl ether acetate, tbp, propylene glycol monomethyl ether, polydimethylsiloxane, methacryloxypropyl silane, dyestuff, after mixing, process 30 ~ 50min with ultrasonic oscillation again, obtain nano-graphite electrically conductive ink.
The mol ratio of the 2,4 toluene diisocyanate described in step 1) and polyoxyethylene glycol is 1.3 ~ 1.4:1.
Step 2) described in the mass ratio of epoxy resin, ethylene glycol ether acetate and isocyanate terminated base polyurethane prepolymer for use as be 9.5 ~ 10:5 ~ 6:1.
The mass ratio of the polyurethane modified epoxy resin described in step 3), graphite, propylene glycol monomethyl ether acetate, tbp, propylene glycol monomethyl ether, polydimethylsiloxane, methacryloxypropyl silane, dyestuff is: 26 ~ 30:5 ~ 6:10 ~ 11:4 ~ 6:5 ~ 7:3 ~ 5:2 ~ 3:5 ~ 8.
Described dyestuff is a kind of in following substances: C.I. is directly black 166, and C.I. is directly black 19, and C.I. is directly black 168, C.I. acid yellow 23, C.I. Xylene Red 52, C.I. acid blue 9.
Beneficial effect of the present invention: the surface effects, the small-size effect that have due to nano-graphite, quantum effect and macro quanta tunnel effect, thus make nano-graphite material there is more excellent physical chemistry and surface and boundary and character compared with conventional blocky graphite material.Nano-graphite electrically conductive ink disclosed by the invention, due to adding of nano-graphite, makes ink have the advantages such as electroconductibility is strong, viscosity is little, fragility is little, elasticity is large, shock-resistance is good.
Embodiment
Embodiment 1
1) by the polyoxyethylene glycol of 10mol, heating vacuumizes dewaters to water-content≤0.2%, inflated with nitrogen protection after being cooled to 20 ~ 25 DEG C, regulate 80 ~ 85 DEG C of interior temperature, add the 2,4 toluene diisocyanate of 13mol, stirring reaction to-NCO content is≤4%, stopped reaction, is cooled to 20 ~ 25 DEG C, obtains isocyanate terminated base polyurethane prepolymer for use as;
2) in reaction, add the epoxy resin of 100g, add again the ethylene glycol ether acetate of 50g to dissolve completely, 75 ~ 80 DEG C of temperature in keeping, then add the isocyanate terminated base polyurethane prepolymer for use as of the 10g that step 1) arrives, reaction 2.5 ~ 3h, obtains polyurethane modified epoxy resin;
3) polyurethane modified epoxy resin of 30g is dissolved in to acetone, adding particle diameter is the 5g graphite of 7～8nm, add again 10g propylene glycol monomethyl ether acetate, 6g tbp, 5g propylene glycol monomethyl ether, 4g polydimethylsiloxane, 2.5g methacryloxypropyl silane, 6g C.I. direct black 166, after mixing, process 30 ~ 50min with ultrasonic oscillation again, obtain nano-graphite electrically conductive ink.
Embodiment 2
1) by the polyoxyethylene glycol of 10mol, heating vacuumizes dewaters to water-content≤0.2%, inflated with nitrogen protection after being cooled to 20 ~ 25 DEG C, regulate 80 ~ 85 DEG C of interior temperature, add the 2,4 toluene diisocyanate of 14mol, stirring reaction to-NCO content is≤4%, stopped reaction, is cooled to 20 ~ 25 DEG C, obtains isocyanate terminated base polyurethane prepolymer for use as;
2) in reaction, add 95g epoxy resin, then add 55g ethylene glycol ether acetate to dissolve completely, keep 75 ~ 80 DEG C of interior temperature, then add the isocyanate terminated base polyurethane prepolymer for use as of 10g, reaction 3h, obtains polyurethane modified epoxy resin;
3) polyurethane modified epoxy resin of 28g is dissolved in to acetone, adding particle diameter is the 6g graphite of 7～8nm, add again the C.I. direct black 19 of 10g propylene glycol monomethyl ether acetate, 4g tbp, 7g propylene glycol monomethyl ether, 3g polydimethylsiloxane, 2g methacryloxypropyl silane, 8g, after mixing, process 45min with ultrasonic oscillation again, obtain nano-graphite electrically conductive ink.
Claims (4)
1. a preparation method for nano-graphite electrically conductive ink, the steps include:
1) by polyoxyethylene glycol, heating vacuumizes dewaters to water-content≤0.2%, inflated with nitrogen protection after being cooled to 20 ~ 25 DEG C, in regulating, 80 ~ 85 DEG C of temperature, add 2,4 toluene diisocyanate, stirring reaction to-NCO content is≤4%, stopped reaction, is cooled to 20 ~ 25 DEG C, obtains isocyanate terminated base polyurethane prepolymer for use as;
2) in reaction, add epoxy resin, then add ethylene glycol ether acetate to dissolve completely, 75 ~ 80 DEG C of temperature in keeping, the more isocyanate terminated base polyurethane prepolymer for use as that adds step 1) to obtain, reaction 2.5 ~ 3h, obtains polyurethane modified epoxy resin;
3) by step 2) polyurethane modified epoxy resin of gained is dissolved in acetone, adding particle diameter is the graphite of 7～8nm, add again propylene glycol monomethyl ether acetate, tributyl phosphate, propylene glycol monomethyl ether, polydimethylsiloxane, methacryloxypropyl silane, dyestuff, after mixing, process 30 ~ 50min with ultrasonic oscillation again, obtain nano-graphite electrically conductive ink;
The mass ratio of the polyurethane modified epoxy resin described in step 3), graphite, propylene glycol monomethyl ether acetate, tributyl phosphate, propylene glycol monomethyl ether, polydimethylsiloxane, methacryloxypropyl silane, dyestuff is: 26 ~ 30:5 ~ 6:10 ~ 11:4 ~ 6:5 ~ 7:3 ~ 5:2 ~ 3:5 ~ 8.
2. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: the mol ratio of the 2,4 toluene diisocyanate described in step 1) and polyoxyethylene glycol is 1.3 ~ 1.4:1.
3. the preparation method of a kind of nano-graphite electrically conductive ink according to claim 1, is characterized in that: step 2) described in the mass ratio of epoxy resin, ethylene glycol ether acetate and isocyanate terminated base polyurethane prepolymer for use as be 9.5 ~ 10:5 ~ 6:1.
4. according to the preparation method of a kind of nano-graphite electrically conductive ink described in the arbitrary claim of claims 1 to 3, it is characterized in that: described dyestuff is a kind of in following substances: C.I. direct black 166, C.I. directly black 19, C.I. directly black 168, C.I. acid yellow 23, C.I. Xylene Red 52, C.I. acid blue 9.
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| CN201210536362.3A CN103102742B (en) | 2012-12-12 | 2012-12-12 | Preparation method of nano graphite conductive ink |
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| CN103102742B true CN103102742B (en) | 2014-09-17 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106147385A (en) * | 2016-08-29 | 2016-11-23 | 苏州安洁科技股份有限公司 | A kind of radio frequency identification system printing conductive ink composition |
| CN106189525A (en) * | 2016-08-29 | 2016-12-07 | 苏州安洁科技股份有限公司 | A kind of electrically conductive ink for RFID antenna printing |
| CN107903714A (en) * | 2017-12-19 | 2018-04-13 | 朱宇浩 | A kind of electrically conductive ink and preparation method thereof |
| CN115595055A (en) * | 2022-10-28 | 2023-01-13 | 昆山威斯泰电子技术有限公司（Cn） | Conductive polyurethane coating, conductive film and preparation method of conductive polyurethane coating |
| CN116285501A (en) * | 2023-02-21 | 2023-06-23 | 华赫技术有限公司 | Preparation method of ink electric conductor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1524881A (en) * | 1975-07-07 | 1978-09-13 | Dick Co Ab | Printing ink |
| CN101528869A (en) * | 2006-06-30 | 2009-09-09 | 录象射流技术公司 | Ink jet ink composition and method for printing |
| CN101824133A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | Preparation method for waterborne polyurethane modified epoxy resin curing agent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7691294B2 (en) * | 2005-03-04 | 2010-04-06 | Inktec Co., Ltd. | Conductive inks and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1524881A (en) * | 1975-07-07 | 1978-09-13 | Dick Co Ab | Printing ink |
| CN101528869A (en) * | 2006-06-30 | 2009-09-09 | 录象射流技术公司 | Ink jet ink composition and method for printing |
| CN101824133A (en) * | 2010-04-28 | 2010-09-08 | 天津大学 | Preparation method for waterborne polyurethane modified epoxy resin curing agent |
Non-Patent Citations (2)
| Title |
|---|
| 导电油墨的制备与性能研究;陈雷;《化学生物与工程》;20080731;第25卷(第7期);第1.2节 * |
| 陈雷.导电油墨的制备与性能研究.《化学生物与工程》.2008,第25卷(第7期),第25-27页. |
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