CN102424379B - Preparation method of high-dispersibility carbon nanotube - Google Patents
Preparation method of high-dispersibility carbon nanotube Download PDFInfo
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- CN102424379B CN102424379B CN2011102790966A CN201110279096A CN102424379B CN 102424379 B CN102424379 B CN 102424379B CN 2011102790966 A CN2011102790966 A CN 2011102790966A CN 201110279096 A CN201110279096 A CN 201110279096A CN 102424379 B CN102424379 B CN 102424379B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 51
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 39
- 239000002253 acid Substances 0.000 claims abstract description 33
- 239000003595 mist Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 230000001590 oxidative effect Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- 101100006584 Mus musculus Clnk gene Proteins 0.000 claims description 22
- 230000004913 activation Effects 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 235000001892 vitamin D2 Nutrition 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 150000007513 acids Chemical class 0.000 abstract 1
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of a high-dispersibility carbon nanotube, comprising the following steps: heating strong oxidizing acids by using a hydrothermal vessel to form acid mist; then activating a carbon nanotube by using the acid mist; processing the activated carbon nanotube in a pressure reaction unit under the conditions of a certain temperature and a certain time to obtain a carbon tube; washing the carbon tube; then drying the washed carbon tube in vacuum to obtain powder; and according to required carbon nanotube dispersion concentration, directly dissolving the powder in relative solvents to obtain the high-dispersibility carbon nanotube.
Description
Technical field
The present invention relates to a kind of preparation method of high-dispersibility carbon nanotube.
Background technology
Carbon nanotube is a kind of very important nano material, and its diameter is generally in a few nanometer to tens nanometers, and length can reach several microns to several millimeters.Since 1991, Japanese scientist Iijima, due to its unique structure and the good characteristics such as electricity, optics and mechanics, was applied in field of nanometer technology since finding carbon nanotube widely.Aspect conductivity, carbon nanotube is identical with the graphite flake layer structure, has good electrology characteristic, can form conductive network; Utilize its nano effect, can electromagnetic wave absorption, reach radiation-resistant effect; Aspect mechanical property, it is 100 times of steel, and density only has 1/6 of steel.Utilize its above performance, the carbon current nanotube all is widely used at aspects such as ultracapacitor, conductive plastics, electromagnetic interference material, stealth material, lithium ion battery, dye sensitization solar battery, support of the catalyst.
Yet, owing to existing the high surface that between extremely strong pipe, Van der Waals force and carbon pipe itself have can between carbon nanotube, be in the thermodynamic instability state, carbon nanotube forms side by side the pencil form mainly with a large amount of single-root carbon nano-tubes and exists, make carbon nanotube almost can not be scattered in all solvents, this has affected the practical application of carbon nanotube greatly.Therefore, how carbon nanotube effectively being dispersed in solvent, is the matter of utmost importance of carbon nanotube application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-dispersibility carbon nanotube, adopt hydro-thermal container heating acid with strong oxidizing property, form the high density acid mist, utilize acid mist to carry out the activation treatment carbon nanotube, process according to certain temperature and time in water heating kettle, obtain the carbon pipe, washing, dry under vacuum condition, obtain powder, carbon nano tube dispersion liquid concentration as required, directly be dissolved in configuration in related solvents and form.Its main thought is: adopt hydro-thermal container heating acid with strong oxidizing property, form the high density acid mist, utilize acid mist to carry out the activation treatment carbon nanotube, process according to certain temperature and time in water heating kettle, obtain the carbon pipe, washing, dry under vacuum condition, obtain powder, carbon nano tube dispersion liquid concentration as required, directly be dissolved in configuration in related solvents and form.
The preparation method of high-dispersibility carbon nanotube of the present invention comprises:
1,0.1-10.0g carbon pipe is put into Glass Containers;
2, container is put into stress reaction device h;
3, add acid with strong oxidizing property or strong base solution in high temperature high pressure device, utilize acid mist or alkali mist and carbon nanotube reaction;
4, pressure reacting container is heated 1-24h under 100-300 ℃ of condition, process the carbon pipe, then oven dry, be dispersed in coordinative solvent according to quality.
Concrete technical scheme is as follows:
A kind of preparation method of high-dispersibility carbon nanotube, adopt following steps:
(1) adopt hydro-thermal container heating acid with strong oxidizing property;
(2) after forming acid mist, utilize acid mist to carry out the activation treatment carbon nanotube;
(3) process according to certain temperature and time in the stress reaction device, obtain the carbon pipe;
(4) the carbon pipe is washed;
(5) then dry under vacuum condition, obtain powder;
(6) as required carbon nano tube dispersion liquid concentration, directly be dissolved in related solvents and obtain high-dispersibility carbon nanotube.
Further, form high density strong oxidizing property acid mist activated carbon pipe in step (2).
Further, described high density strong oxidizing property acid mist is removed carbon tube-surface impurity, cuts off the carbon pipe, and on its surface, forms carboxyl, thereby makes the carbon pipe have good dispersiveness.
Further, step (1) also comprises before: the carbon pipe is put into Glass Containers, the Glass Containers container is put into the stress reaction device.
Further, step (3) is further for to heat 1-24h with the stress reaction device under 100-300 ℃ of condition.
Further, described stress reaction device is water heating kettle.
Further, take in the thin mouthful of vial that the untreated carbon nanotube of 0.100g is positioned in advance the 10ml that cleans, phial is put into the white reaction still of 50ml except decap.
Further, the gap location at vial and white reaction kettle adds appropriate concentrated nitric acid, sealing kettle and steel bushing, then 250 ℃ of activation 24h in baking oven.
Further, the concentrated nitric acid add-on is lower than the glass bottle opening height.
Further, carry out vacuum-drying at 60 ℃ in step (5).
Compare with currently available technology, the present invention proposes a kind of preparation method of high-dispersibility carbon nanotube, adopt hydrothermal method to form strong oxidizing property acid mist activated carbon pipe, except carbon elimination tube-surface impurity, cut off the carbon pipe, and on its surface, form carboxyl, thereby make the carbon pipe have good dispersiveness.Due in conventional processing, most of a large amount of acid or a small amount of carbon nanotube of dipping by lye, environmental pollution weight of adopting.Adopt the strong acid atomization of minute quantity to process the carbon pipe in the present invention, and disperse, reduce the consumption and the pollution that reduces environment of acid, have good economic and social benefit.
Description of drawings
Fig. 1 is acid mist method activated carbon plumber skill diagram
Fig. 2 is the SEM picture of carbon pipe after the acid mist method is processed
Fig. 3 is: the aqueous dispersion liquid of 2mg/ml carbon nanotube (A), the aqueous dispersion liquid of 10mg/ml carbon nanotube (B), the ethanol phase dispersant liquid (C) of 2mg/ml carbon nanotube, the ethylene glycol phase dispersant liquid (D) of 2mg/ml carbon nanotube
Embodiment
Below describe the present invention with reference to the accompanying drawings, it is a kind of preferred embodiment in numerous embodiments of the present invention.
Method one: the method comprises the following steps:
1, take in the thin mouthful of vial that the untreated carbon nanotube of 0.100g is positioned in advance the 10ml that cleans;
2, phial is put into the white reaction still (seeing figure one) of 50ml except decap;
3, add appropriate concentrated nitric acid (lower than the glass bottle opening height) at the gap location of vial and kettle, sealing kettle and steel bushing, then 250 ℃ of activation 24h (acid mist that produces while utilizing high temperature, etching carbon pipe) in baking oven;
4, reacted carbon pipe is repeatedly washed suction filtration, 60 ℃ of vacuum-dryings;
5, carbon pipe after activation is configured to the dispersion liquid of different concns, different solvents according to demand.
Method two: the method comprises the following steps:
1, take in the thin mouthful of vial that the untreated carbon nanotube of 1.000g is positioned in advance the 10ml that cleans;
2, phial is put into the white reaction still of 100ml except decap;
3, add appropriate concentrated nitric acid (lower than the glass bottle opening height) at the gap location of vial and kettle, sealing kettle and steel bushing, then 200 ℃ of activation 10h (acid mist that produces while utilizing high temperature, etching carbon pipe) in baking oven;
4, reacted carbon pipe is repeatedly washed suction filtration, 60 ℃ of vacuum-dryings;
5, carbon pipe after activation is configured to the dispersion liquid of different concns, different solvents according to demand.
Method three: the method comprises the following steps:
1, take in the thin mouthful of vial that the untreated carbon nanotube of 10.0g is positioned in advance the 50ml that cleans;
2, phial is put into the white reaction still of 500ml except decap;
3, add appropriate concentrated nitric acid (lower than the glass bottle opening height) at the gap location of vial and kettle, sealing kettle and steel bushing, then 100 ℃ of activation 24h (acid mist that produces while utilizing high temperature, etching carbon pipe) in baking oven;
4, reacted carbon pipe is repeatedly washed suction filtration, 60 ℃ of vacuum-dryings;
5, carbon pipe after activation is configured to the dispersion liquid of different concns, different solvents according to demand.
As can be known, can be dispersed in inorganic and organic phase with different concns by the carbon nanotube after the acid mist activation treatment, and carbon nanotube dispersed is even, forms stable dispersion liquid, helps the further application of carbon nanotube from figure three.
The carbon nanotube that application acid mist method is processed, surface ratio is cleaner, and become single distribution, the consistent appearance of product is better, and method is simple, easy handling, in carbon nanotube activation dispersion process, need not to use other dispersion agent, only respective quality carbon pipe need to be dispersed in corresponding solvent, ultra-sonic dispersion gets final product.In the activation of carbon pipe, adopt a small amount of sour high-temperature atomizing, fully process carbon nanotube, namely saved sour consumption, also reduce the aftertreatment of remaining acid solution, have economy and the social effect of environmental protection.
The above is exemplarily described the present invention by reference to the accompanying drawings; obviously specific implementation of the present invention is not subject to the restrictions described above; as long as the various improvement of having adopted method design of the present invention and technical scheme to carry out; or without improvement, directly apply to other occasion, all within protection scope of the present invention.
Claims (6)
1. the preparation method of a high-dispersibility carbon nanotube, is characterized in that, the carbon pipe is put into Glass Containers, and Glass Containers is put into the stress reaction device, and adopt following steps:
(1) adopt hydro-thermal container heating acid with strong oxidizing property;
(2) after forming acid mist, utilize acid mist to carry out activation treatment carbon pipe, form high density strong oxidizing property acid mist activated carbon pipe, described high density strong oxidizing property acid mist is removed carbon tube-surface impurity, cut off the carbon pipe, and on its surface, form carboxyl, thereby make the carbon pipe have good dispersiveness;
(3) the stress reaction device is heated 1-24h under 100-300 ℃ of condition, obtain the carbon pipe;
(4) the carbon pipe is washed;
(5) then dry under vacuum condition, obtain powder;
(6) as required carbon nano tube dispersion liquid concentration, directly be dissolved in related solvents and obtain high-dispersibility carbon nanotube.
2. the preparation method of high-dispersibility carbon nanotube as claimed in claim 1, is characterized in that, described stress reaction device is water heating kettle.
3. the preparation method of high-dispersibility carbon nanotube as claimed in claim 1, is characterized in that, takes in the thin mouthful of vial that the untreated carbon pipe of 0.100g is positioned in advance the 10ml that cleans, and thin mouthful of vial put into the white reaction still of 50ml except decap.
4. the preparation method of high-dispersibility carbon nanotube as claimed in claim 3, is characterized in that, at the gap location of thin mouthful of vial and white reaction kettle, adds appropriate concentrated nitric acid, sealing kettle and steel bushing, then 250 ℃ of activation 24h in baking oven.
5. the preparation method of high-dispersibility carbon nanotube as claimed in claim 4, is characterized in that, the concentrated nitric acid add-on is lower than thin mouthful of glass bottle opening height.
6., as the preparation method of the described high-dispersibility carbon nanotube of any one in claim 1-5, it is characterized in that, step is carried out vacuum-drying at 60 ℃ in (5).
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| CN2011102790966A CN102424379B (en) | 2011-09-20 | 2011-09-20 | Preparation method of high-dispersibility carbon nanotube |
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| CN102424379B true CN102424379B (en) | 2013-11-20 |
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| CN104724691B (en) * | 2013-12-23 | 2016-11-09 | 北京阿格蕾雅科技发展有限公司 | A kind of method improving SWCN dispersiveness |
| CN104724692B (en) * | 2013-12-23 | 2016-11-16 | 北京阿格蕾雅科技发展有限公司 | The homodisperse method of SWCN |
| CN105806674A (en) * | 2016-03-08 | 2016-07-27 | 武汉水天成环保科技有限公司 | Preparation method of acid nanoparticles for calibration |
| CN108517006B (en) * | 2018-05-10 | 2021-05-28 | 暨南大学 | Polypeptide material for improving dispersibility of carbon nano tube in water under normal temperature and pressure condition and application thereof |
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| EP1061042A1 (en) * | 1999-06-15 | 2000-12-20 | Iljin Nanotech Co., Ltd. | Method for gas phase purification of carbon nanotubes by thermal treatment in diffusion furnace |
| CN1397488A (en) * | 2001-07-18 | 2003-02-19 | 中国科学院成都有机化学研究所 | Post-processing process for increasing specific surface area of carbon nanotube |
| DE102008031579A1 (en) * | 2008-07-03 | 2010-01-07 | Bayer Materialscience Ag | A highly efficient gas phase process for the modification and functionalization of carbon nanofibers with nitric acid vapor |
| CN102153069B (en) * | 2011-02-25 | 2012-12-19 | 中国科学院长春应用化学研究所 | Treatment method for nanometer carbon material |
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