CN108690403A - A kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink - Google Patents
A kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink Download PDFInfo
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- CN108690403A CN108690403A CN201710236252.8A CN201710236252A CN108690403A CN 108690403 A CN108690403 A CN 108690403A CN 201710236252 A CN201710236252 A CN 201710236252A CN 108690403 A CN108690403 A CN 108690403A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The present invention relates to a kind of silicon rubber base wear-resistant conductive graphenes to print ink, and the mass fraction group of each component becomes:10~100 parts of the graphene that 100 parts of silicon rubber, 1~5 parts of atmospheric oxidising organic compound containing unsaturated group, 200~500 parts of volatile organic solvent, 0.01~1.5 part of catalyst, 1~10 part of crosslinking agent, 0.2~3 part of caking property additive, 0.2~3 part of caking property accelerating agent, cladding are handled.Graphene is the one or more of single-layer or multi-layer and piece diameter in 0.001 μm~5 μm graphenes.The present invention also provides the methods for preparing above-mentioned Graphene conductive ink.Preparation process of the present invention is simple, of low cost, and ink stability is good, electric conductivity is excellent, mobility is good;There is preferable mechanicalness, pressing mold, cementability, impact resilience, wearability and scratch resistance after ink molding.Graphene is handled by silicones cladding, and cladding processing silicones includes the one or more of methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones, improves graphene mechanical property and stably dispersing performance in ink.
Description
Technical field
The present invention relates to a kind of preparation methods of printing ink, more specifically to a kind of silicon rubber base wear-resistant conductive
Property graphene printing ink preparation method.
Background technology
In modern printing technology, by using conductive ink print, word, Ke Yipai on insulation stock
It destatics, is conductive.Nowadays electrically conductive ink mainly have gold system conductive ink, silver system conductive ink, copper system conductive ink Oh, carbon series conductive ink
Etc. several classes, and to reach practical.Gold system conductive ink possesses the advantage that bronze chemical property is stable, conducts electricity very well, still
Expensive, purposes is only limitted to rear vlsi die;Silver system conductive ink is largely used to the conductive printing of flexible circuit board, has and leads
Good electrical property, the advantages that having a wide range of application, but it is expensive, temperature sensitive, for resistance value by temperature change, fluctuation is larger;
Copper system conductive ink is cheap, but is oxidized easily in use there are copper powder and the fatal of electric conductivity decline is caused to lack
Point;Graphite, carbon fiber, cost of carbon black are relatively low in carbon series conductive ink, but its electric conductivity is general, and sheet resistance value is far above silver
It is conductive ink, and the mechanical performance of ink, resistance to stripping, scraping and wiping resistance performance are poor.The binder of ink would generally select polyurethane, ring
Oxygen resin, phenolic resin.
Graphene as a newcomer in carbon nanomaterial, have high conductivity, high intensity, high electron mobility,
The advantages such as flexible, infiltration particle channel, are applied to the preparation of novel conductive ink, have broad prospects.Graphene/poly-
Close object nanocomposite electrically conductive ink have higher conductivity, more preferably mechanical strength, lighter quality and it is cheap at
This, compared to the Prospect of R & D and market value that the conventional conductives ink such as nano metal system have bigger.Graphene/polymer nanocomposite
Composite material conductive ink is at present there is also many problems, for example the dispersibility of graphene poor lead to the stability of ink and makes
It is poor with property.
Therefore develop that a kind of graphene dispersion is good and the good Graphene conductive ink of stability in use is current
Urgent problem to be solved.
Invention content
The purpose of the present invention is be directed to above-mentioned present situation, it is desirable to provide a kind of graphene printing ink preparation having good stability
Method.
The object of the invention is achieved in that, an a kind of preparation side for silicon rubber base wear-resistant conductive graphene printing ink
Method, preparation are as follows:
1) 100 parts of graphene powders are weighed, with silicones/carbitol acetate ester solution impregnation, ball mill is transferred to or grinds
Grinding machine is ground, and is cleaned, and is dried at room temperature for obtaining the graphene powder of silicones cladding processing;The graphene powder is single layer
Or multilayer and piece diameter are in the one or more of 0.001~5 μm of graphene;Silicones is methyl phenyl silicone resin, vinyl silicon tree
The one or more of fat, methyl hydrogen silicones;
2) 100 parts of silicon rubber are weighed, the graphene powder that 10~100 parts of step 1) silicones claddings are handled, it is low under normal temperature and pressure
Speed 0.5~1h of stirring, high speed stirs 2~3h and obtains base-material under then being depressurized at 100~150 DEG C, after being cooled to room temperature, upwards
200~500 parts of volatile organic solvents of addition in base-material are stated, are repeatedly divided using three-roll grinder grinding after stirring evenly
Dispersion liquid;The silicon rubber is one kind or more of Methyl-ethylenvinyl gum, Vinyl MQ silicon resin, vinyl polysiloxane
Kind;The volatile organic solvent be toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, hexadecane and
Ring hexadecane.
3) 0.05 part~2 parts catalyst, 1~10 part of crosslinking agent, 1~3 part of air oxygen are added in the dispersion liquid of step 2)
The property changed organic compound containing unsaturated group, 0.2~3 part of caking property additive, 0.2~3 part of caking property accelerating agent, after mixing
It is ground repeatedly using three-roll grinder and silicon rubber base wear-resistant conductive graphene is obtained by filtration and print ink;The crosslinking agent
Methylhydrogenpolysi,oxane, methyl blocking methylhydrogenpolysi,oxane, phenyl hydrogen-containing silicon oil, methyl hydrogen MQ silicon trees are blocked for reactive hydrogen
Fat, the MQ silicones of hydrogen containing phenyl methyl etc.;The catalyst is platinum-vinyl siloxane composition catalyst, chloroplatinic acid-catalysis
Agent, alcohol are modified chloroplatinic acid catalyst, platinum-alkynes basigamy mixture catalyst etc.;It is described atmospheric oxidising to organise containing unsaturated group
It is preferably tung oil to close object;The caking property additive be vinyltrimethoxysilane, glycidoxy-propyltrimethoxy silane,
Polysiloxane containing epoxy group;The caking property accelerating agent is polysilicon acid methyl esters, ethyl polysilicate one or two.
Advantages of the present invention:
1, processing graphene is simply coated with silicones, improves the compatibility of graphene, graphene can be dispersed in oil
Mo Zhong can form conduction under low filling;
2, atmospheric oxidising organic compound containing unsaturated group is introduced, resistance to stripping, the scraping and wiping resistance performance of ink are improved;
3, using silicon rubber as bridging agent so that mechanical performance is preferably and with certain flexibility after electrically conductive ink molding;
4, polysilicates is introduced as caking property accelerating agent, improves the adhesive property of ink and base material.
Specific implementation mode
Embodiment 1 weighs 50 parts of graphene powders, with phenyl MQ silicones/carbitol acetate ester solution impregnation, turns
Grinder grinding is moved, is cleaned, is dried at room temperature for obtaining the graphene powder of phenyl MQ silicones cladding processing;In kneader
Viscosity 5000000cps methyl under the bis- envelope vinyl polysiloxane of viscosity 500cps, 10 parts of room temperature is added under 50 parts of room temperature
The graphene powder that vinyl silicon kautschuk, 10 parts of Vinyl MQ silicon resins, 50 parts of above-mentioned silicones claddings are handled, room temperature are normal
0.5~1h of stirring at low speed is depressed, high speed stirs 2~3h and obtains base-material under then being depressurized at 100~150 DEG C, and slurry is in three rollers
It is ground 2-3 times on grinder, after being cooled to room temperature, dilution with toluene is added into above-mentioned base-material, using three rollers after stirring evenly
Grinder grinds 2-3 times and obtains dispersion liquid,;It is transferred in planetary stirrer, 0.05 part~2 parts platinum-vinyl siloxanes is added
Composition catalyst, 1~10 part of methyl hydrogen polysiloxane, 1~3 part of tung oil, 0.2~3 part of caking property additive, caking property
0.2~3 part of accelerating agent grinds repeatedly using three-roll grinder after mixing 3~5h and silicon rubber base wear-resistant conductive is obtained by filtration
Property graphene print ink.
Embodiment 2, with embodiment 1, unlike, add 50 parts of claddings treated that graphene powder replaces with addition 70
Part cladding treated graphene powder.
Embodiment 3, with embodiment 1, unlike, add 50 parts of claddings treated that graphene powder replaces with addition
100 parts of cladding treated graphene powders.
Comparative example 1, with embodiment 1, unlike, graphene powder is without any processing.
Comparative example 2 weighs 50 parts of graphene powders, with phenyl MQ silicones/carbitol acetate ester solution impregnation, turns
Grinder grinding is moved, is cleaned, is dried at room temperature for obtaining the graphene powder of phenyl MQ silicones cladding processing;In kneader
Viscosity 5000000cps methyl under the bis- envelope vinyl polysiloxane of viscosity 500cps, 10 parts of room temperature is added under 50 parts of room temperature
The graphene powder that vinyl silicon kautschuk, 10 parts of Vinyl MQ silicon resins, 50 parts of above-mentioned silicones claddings are handled, room temperature are normal
0.5~1h of stirring at low speed is depressed, high speed stirs 2~3h and obtains base-material under then being depressurized at 100~150 DEG C, and slurry is in three rollers
It is ground 2-3 times on grinder, after being cooled to room temperature, dilution with toluene is added into above-mentioned base-material, using three rollers after stirring evenly
Grinder grinds 2-3 times and obtains dispersion liquid,;It is transferred in planetary stirrer, 0.05 part~2 parts platinum-vinyl siloxanes is added
Composition catalyst, 1~10 part of methyl hydrogen polysiloxane, 0.2~3 part of caking property additive, caking property accelerating agent 0.2~
It 3 parts, is ground repeatedly using three-roll grinder after mixing 3~5h and the printing of silicon rubber base wear-resistant conductive graphene is obtained by filtration
Ink.
By the various embodiments described above gained Graphene conductive ink by being screen printed onto on base material, film thickness is about 50 μm, room
To its fineness, adhesive force and resistivity measurement after temperature solidification, test result is as follows shown in table:
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Fineness/μm | ≤10 | ≤10 | ≤10 | ≤10 | ≤10 |
| Adhesive force(Cross-hatching) | 100/100 | 100/100 | 100/100 | 100/100 | 100/100 |
| Resistivity/Ω cm | 2.1 | 1.7 | 0.5 | 27 | 2.2 |
By Graphene conductive ink obtained by the various embodiments described above by being screen printed onto lettering on base material, room temperature curing be thickness about
For 40 μm of label, then sand erasing rubber is used to evaluate wearability, test result is as follows shown in table:
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Erasing times | 3513 | 3013 | 2755 | 1832 | 1756 |
As can be seen that the silicon rubber based printing ink of silicones cladding processing graphene preparation is relatively low in loading from above-mentioned table
In the case of have a good electric conductivity, graphene improves the wear-resisting property of shaping membrane by silicones cladding post-processing,
Caking property agent and adhesive accelerant improve shaping membrane adhesive force, and the addition of atmospheric oxidising unsaturated organic compound obviously changes
It has been apt to the wearability of shaping membrane.
Claims (5)
1. a kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink, it is characterised in that:It is as follows:
1) 100 parts of graphene powders are weighed, with silicones/carbitol acetate ester solution impregnation, ball mill is transferred to or grinds
Grinding machine is ground, and is cleaned, and is dried at room temperature for obtaining the graphene powder of silicones cladding processing;
The graphene powder is the one or more of single-layer or multi-layer and piece diameter in 0.001~5 μm of graphene;
Silicones is the one or more of methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones;
2) 100 parts of silicon rubber are weighed, the graphene powder that 10~100 parts of step 1) silicones claddings are handled, is obtained after stirring evenly
Base-material is obtained, then, 200~500 parts of volatile organic solvents is added into above-mentioned base-material, is ground using three rollers after stirring evenly
Machine grinding repeatedly obtains dispersion liquid;
The silicon rubber be Methyl-ethylenvinyl gum, Vinyl MQ silicon resin, vinyl polysiloxane it is one or more;
The volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, hexadecane
And ring hexadecane.
2.3) 0.05 part~2 parts catalyst, 1~10 part of crosslinking agent, 1~3 part of air oxidation are added in the dispersion liquid of step 2)
Property organic compound containing unsaturated group, 0.2~3 part of caking property additive, 0.2~3 part of caking property accelerating agent, after mixing again
It is ground repeatedly by three-roll grinder and silicon rubber base wear-resistant conductive graphene is obtained by filtration and print ink;
The crosslinking agent be reactive hydrogen block methylhydrogenpolysi,oxane, methyl blocking methylhydrogenpolysi,oxane, phenyl hydrogen-containing silicon oil,
Methyl hydrogen MQ silicones, the MQ silicones of hydrogen containing phenyl methyl etc.;
The catalyst is platinum-vinyl siloxane composition catalyst, chloroplatinic acid catalyst, alcohol are modified chloroplatinic acid catalyst,
Platinum-alkynes basigamy mixture catalyst etc.;
The preferred tung oil of atmospheric oxidising organic compound containing unsaturated group;
The caking property additive is vinyltrimethoxysilane, glycidoxy-propyltrimethoxy silane, gathers containing epoxy group
Organosiloxane;
The caking property accelerating agent is polysilicon acid methyl esters, ethyl polysilicate one or two.
3. a kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink according to claim 1, special
Sign is:Graphene powder described in step 1) is single-layer or multi-layer and piece diameter in one kind of 0.001~5 μm of graphene or several
It plants and passes through the processing of silicones cladding;Cladding is methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones with silicones
Deng;Step 2) the volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, positive ten
Six alkane and ring hexadecane.
4. a kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink according to claim 1, special
Sign is:The agitating mode of base-material is 0.5~1h of stirring at low speed under normal temperature and pressure in step 2), is then depressurized at 100~150 DEG C
Lower high speed stirs 2~3h, and last base-material adds organic solvent mixing after being cooled to room temperature.
5. a kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink according to claim 1, special
Sign is:Caking property additive described in step 3) be vinyltrimethoxysilane, glycidoxy-propyltrimethoxy silane,
Polysiloxane containing epoxy group;The caking property accelerating agent is polysilicon acid methyl esters, ethyl polysilicate one or two.
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| CN201710236252.8A CN108690403A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink |
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| CN201710236252.8A CN108690403A (en) | 2017-04-12 | 2017-04-12 | A kind of preparation method of silicon rubber base wear-resistant conductive graphene printing ink |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205843A (en) * | 2019-06-17 | 2019-09-06 | 浙江海印数码科技有限公司 | A kind of preparation method for the graphene oxide ink-jet ink that Hyperbranched polysilane is modified |
| CN112325762A (en) * | 2020-09-14 | 2021-02-05 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN114276047A (en) * | 2021-12-31 | 2022-04-05 | 武汉中科先进技术研究院有限公司 | High-strength wear-resistant friction material and preparation method thereof |
-
2017
- 2017-04-12 CN CN201710236252.8A patent/CN108690403A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205843A (en) * | 2019-06-17 | 2019-09-06 | 浙江海印数码科技有限公司 | A kind of preparation method for the graphene oxide ink-jet ink that Hyperbranched polysilane is modified |
| CN112325762A (en) * | 2020-09-14 | 2021-02-05 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN112325762B (en) * | 2020-09-14 | 2021-10-01 | 兰州大学 | Graphene multifunctional thin film sensor and preparation method thereof |
| CN114276047A (en) * | 2021-12-31 | 2022-04-05 | 武汉中科先进技术研究院有限公司 | High-strength wear-resistant friction material and preparation method thereof |
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