Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of carbon nano tube dispersion liquid, wherein, carbon nano tube dispersion liquid comprises carbon nano-tube, high conductive black, dispersant and solvent, dispersion liquid homogeneous, stable, high conformity, and in dispersion liquid, contain high conductive black, carbon nanotube conducting network is further improved, further improves the performance of carbon nano tube dispersion liquid.
It is benchmark that the weight percentage of carbon nano tube dispersion liquid is preferably take in the present invention, and described carbon nano tube dispersion liquid comprises the carbon nano-tube of 2.0-6.0wt%, the high conductive black of 2.0-6.0wt%, the dispersant of 0.4-1.0wt% and the solvent of 88-94wt%.
Preferably, high conductive black is the high conductive black that oil factor is larger, and concrete can be greater than 100M for oil factor
2the high conductive black of/g.
Wherein, carbon nano-tube the present invention is restriction not, and preferably carbon nano-tube is multi-walled carbon nano-tubes, and further preferably the caliber of carbon nano-tube is 30nm-60nm, and the pipe range of carbon nano-tube is 5 μ m-20 μ m.
Dispersant preferred dispersants of the present invention is nonionic surface active agent, and concrete can be PVP.
Solvent the present invention can be also water for organic solvent, and preferred solvent of the present invention is 1-METHYLPYRROLIDONE or pure water.
The present invention provides a kind of preparation method of carbon nano tube dispersion liquid simultaneously, and step comprises: carbon nano-tube, high conductive black and dispersant are scattered in solvent, grind to obtain carbon nano tube dispersion liquid.
Wherein, carbon nano-tube, high conductive black and dispersant add the order the present invention in solvent to add by the mode of solvent, carbon nano-tube, dispersant, high conductive black, also can adjust according to actual conditions.
Preferentially, the temperature of grinding is 20 ℃ to 60 ℃, further improves the performance of carbon nano tube dispersion liquid, can avoid high temperature to cause the reunion again of the carbon nano-tube of dispersion.
Preferably, step comprises: in S1, the environment in humidity lower than 30%R.Hs, partial solvent 1-METHYLPYRROLIDONE is packed in basket type sand mill, then add carbon nano-tube, low frequency stirs the wetting carbon nano-tube of 5-10min, rear high frequency sand milling 0.5-1h.S2, the dispersant solution of residual solvent 1-METHYLPYRROLIDONE and polyethylene of dispersing agent base pyrrolidones configuration is packed in above-mentioned basket type sand mill, control 20 ℃~60 ℃ of sand milling temperature, high frequency sand milling 1-2h.S3, high conductive black is packed in above-mentioned basket type sand mill, high frequency sand milling 5-7h makes carbon nano tube dispersion liquid.
Concrete can be:
S1: under normal-temp .-dehumidifying environment (humidity is lower than 30%R.Hs), solvent 1-METHYLPYRROLIDONE is poured in basket type sand mill, and additionally reserved enough solvents are used for dissolving polyethylene of dispersing agent base pyrrolidones.Polyethylene of dispersing agent base pyrrolidones is slowly poured in reserved solvent and do not stopped stirring at low speed wiring solution-forming, and it is limpid and slightly light yellow that standing rear dispersant solution is.
S2: open 20 ℃ of cooling circulating waters, make in sand grinding process slurry temperature between 20 ℃~60 ℃, carbon nano-tube is poured in the solvent in basket type sand mill, and it is wetting with 10Hz low frequency, to stir 5-10min quickening carbon nano-tube, promote subsequently sand milling basket and carry out putting down sand milling basket after scraping, with 35Hz, carry out sand milling 0.5-1h.
S3: the dispersant solution preparing is poured in basket type sand mill, carried out sand milling 1-2h with 35Hz.
S4: high conductive black is poured in basket type sand mill, carried out sand milling 5-7h with 40Hz.
S5: carry out fineness test with Hegman grind gage, make required carbon nano tube dispersion liquid when following when slurry fineness show value reaches 4 μ m.
Or preferably, step comprises: under S1, normal temperature, partial solvent water is packed in basket type sand mill, then add carbon nano-tube, low frequency stirs the wetting carbon nano-tube of 5-10min, rear high frequency sand milling 0.5-1h.S2, the dispersant solution of residual solvent water and polyethylene of dispersing agent base pyrrolidones configuration is packed in above-mentioned basket type sand mill, control 20 ℃~60 ℃ of sand milling temperature, high frequency sand milling 3-4h.S3, high conductive black is packed in above-mentioned basket type sand mill, high frequency sand milling 5-7h makes carbon nano tube dispersion liquid.
Concrete can be:
S1: under normal temperature, solvent pure water is poured in basket type sand mill, and additionally reserved enough solvents are used for dissolving polyethylene of dispersing agent base pyrrolidones.Polyethylene of dispersing agent base pyrrolidones is slowly poured in reserved solvent and do not stopped stirring at low speed wiring solution-forming, and it is limpid and slightly light yellow that standing rear dispersant solution is.
S2: open 20 ℃ of cooling circulating waters, make in sand grinding process slurry temperature between 20 ℃~60 ℃, carbon nano-tube is poured in the solvent in basket type sand mill, and it is wetting with 10Hz low frequency, to stir 5-10min quickening carbon nano-tube, promote subsequently sand milling basket and carry out putting down sand milling basket after scraping, with 35Hz, carry out sand milling 0.5-1h.
S3: the dispersant solution preparing is poured in basket type sand mill, carried out sand milling 3-4h with 35Hz.
S4: high conductive black is poured in basket type sand mill, carried out sand milling 5-7h with 40Hz.
S5: carry out fineness test with Hegman grind gage, make required carbon nano tube dispersion liquid when following when slurry fineness show value reaches 4 μ m.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1-4
(1): under normal-temp .-dehumidifying environment (humidity is lower than 30%R.Hs), solvent 1-METHYLPYRROLIDONE is poured in basket type sand mill, and additionally reserved enough solvents are used for dissolving polyethylene of dispersing agent base pyrrolidones.Polyethylene of dispersing agent base pyrrolidones is slowly poured in reserved solvent and do not stopped stirring at low speed wiring solution-forming, and it is limpid and slightly light yellow that standing rear dispersant solution is.
(2): open 20 ℃ of cooling circulating waters, make in sand grinding process slurry temperature between 20 ℃~60 ℃, carbon nano-tube is poured in the solvent in basket type sand mill, and it is wetting with 10Hz low frequency, to stir 5-10min quickening carbon nano-tube, promote subsequently sand milling basket and carry out putting down sand milling basket after scraping, with 35Hz, carry out sand milling 0.5-1h.
(3): the dispersant solution preparing is poured in basket type sand mill, with 35Hz, carried out sand milling 1-2h.
(4): high conductive black is poured in basket type sand mill, with 40Hz, carried out sand milling 5-7h.
(5): with Hegman grind gage, carry out fineness test, when slurry fineness show value reaches 4 μ m, make below carbon nano tube dispersion liquid sample S1-S4.
Wherein, the raw material using in said method is as follows respectively:
Embodiment 1
Embodiment 2
Embodiment 3
Embodiment 4
Embodiment 5-8
(1): under normal temperature, solvent pure water is poured in basket type sand mill, and additionally reserved enough solvents are used for dissolving polyethylene of dispersing agent base pyrrolidones.Polyethylene of dispersing agent base pyrrolidones is slowly poured in reserved solvent and do not stopped stirring at low speed wiring solution-forming, and it is limpid and slightly light yellow that standing rear dispersant solution is.
(2): open 20 ℃ of cooling circulating waters, make in sand grinding process slurry temperature between 20 ℃~60 ℃, carbon nano-tube is poured in the solvent in basket type sand mill, and it is wetting with 10Hz low frequency, to stir 5-10min quickening carbon pipe, promote subsequently sand milling basket and carry out putting down sand milling basket after scraping, with 35Hz, carry out sand milling 0.5-1h.
(3): the dispersant solution preparing is poured in basket type sand mill, with 35Hz, carried out sand milling 3-4h.
(4): high conductive black is poured in basket type sand mill, with 40Hz, carried out sand milling 5-7h.
(5): with Hegman grind gage, carry out fineness test, when slurry fineness show value reaches 4 μ m, make below carbon nano tube dispersion liquid sample S5-S8.
Wherein, the raw material using in said method is as follows respectively:
Embodiment 5:
Embodiment 6
Embodiment 7
Embodiment 8:
Comparative example 1
Raw material: 30nm-60nm caliber carbon nano-tube-9.4%
PVP-0.6%
1-METHYLPYRROLIDONE-90%
Carbon nano-tube, PVP are joined in 1-METHYLPYRROLIDONE to the ultrasonic dispersion of 40Hz 10h at 50 ℃ and make carbon nano tube dispersion liquid sample DS1.
Comparative example 2
Raw material: 30nm-60nm caliber carbon nano-tube-8.0%
PVP-0.6%
Pure water-91.4%
Carbon nano-tube, the PVP ultrasonic dispersion of the 40Hz 12h at 50 ℃ that is added to the water is made to carbon nano tube dispersion liquid sample DS2.
Performance test
Dispersed, stability: checkout equipment, adopt (Shanghai rib light) ultraviolet specrophotometer, model 752s, selects wavelength 800nm, blank sample is NMP(N-methyl pyrrolidone).Carbon nano tube dispersion liquid sample S1-S8 and DS1-DS2 are tested, and test result is as table 1.
Fineness: normative reference, fineness gauge determination method GB172479; Checkout equipment, the Central Asia, Tianjin QXD-25 type Hegman grind gage; Testing conditions, 22 ± 1 ℃ of room temperatures, relative humidity 70%R.H; Detecting step, 1. with alcohol, clean scraper plate and scraper, and with cotton yarn dry 2. with glass bar dip in a little even testing sample splash into slot scraping bosom 3. both hands in being pulled through 4. for 5 seconds by deep trouth place to shallow place with scraper on scraper plate, observe groove endoparticle and evenly appear place, corresponding numerical value is grain fineness.Carbon nano tube dispersion liquid sample S1-S8 and DS1-DS2 are tested, and test result is as table 1.
SEM test: normative reference, GB/T17359-1998, GB/T16594-1996, JY/T010-1996; Accelerating voltage: 5.0KV, tests carbon nano tube dispersion liquid sample S2, S3, S5, S7 and DS1, DS2, and test result is as accompanying drawing 1-6.
Table 1
Sample |
Fineness (μ m) |
Stability (%) |
Dispersed |
S1 |
2.8 |
83.2 |
1.478 |
S2 |
2.5 |
81.7 |
1.327 |
S3 |
2.6 |
84.1 |
1.566 |
S4 |
2.5 |
82.7 |
1.521 |
S5 |
3.0 |
84.6 |
1.393 |
S6 |
2.6 |
87 |
1.185 |
S7 |
2.8 |
85.2 |
1.468 |
S8 |
3.0 |
83.3 |
1.507 |
DS1 |
4.7 |
64.1 |
0.832 |
DS2 |
4.2 |
61.7 |
0.694 |
Carbon nano tube dispersion liquid homogeneous of the present invention, stable, high conformity; carbon nano tube dispersion liquid of the present invention only needs to dispersible by conventional grinding; its preparation more simply, more practical; in preparation method of the present invention, disperseing only needs can complete by cheap milling apparatus; and rate of finished products is high, security performance is good, simple to operate, efficiency is high, can greatly reduce dispersion cost, improves the quality of products; batch production preferably, is suitable for the production application of large-scale.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.