CN100491240C - Photochemical carbon nanotube modifying process - Google Patents
Photochemical carbon nanotube modifying process Download PDFInfo
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- CN100491240C CN100491240C CNB2006101188935A CN200610118893A CN100491240C CN 100491240 C CN100491240 C CN 100491240C CN B2006101188935 A CNB2006101188935 A CN B2006101188935A CN 200610118893 A CN200610118893 A CN 200610118893A CN 100491240 C CN100491240 C CN 100491240C
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- carbon nanotube
- benzhydrol
- photochemical
- benzophenone
- modifying
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Abstract
The present invention discloses a kind of photochemical carbon nanotube modifying process, and belongs to the field of nanometer technology. The process includes the following steps: mixing carbon nanotube, benzophenone and diphenyl carbinol in organic solvent to form mixed solution; ultrasonic treatment of the mixed solution; irradiating the mixed solution with ultrasonic ray while stirring to react; washing the product with organic solvent; and drying to obtain the functional carbon nanotube. The process is simple and effective, and the obtained functional carbon nanotube may be well dispersed in organic solvent for reaction with other compound and for preparing nanometer composite material.
Description
Technical field
What the present invention relates to is the method for a kind of method of field of nanometer technology, particularly a kind of photochemical carbon nanotube modifying.
Background technology
Carbon nanotube is because its unique physics and chemical property since being found, have just caused the great interest of people.For the strong Van der Waals that overcomes between the carbon nanotube interacts, improve the dispersing property of carbon nanotube in solvent, perhaps strengthen the interaction between it and the other materials, it is very important means that carbon nano tube surface is modified.
Find through literature search prior art, at present with photochemistry carbon nano tube modified method is had two kinds: people such as Micheal Holzinger are in " Angewandte Chemie International Edition " (" German applied chemistry ", 2001,40 phases, the 4002-4005 page) deliver the paper that is entitled as " Sidewallfunctionalization of carbon nanotubes " (" functionalization of carbon nanotube tube wall "), the method for a kind of usefulness 17 fluoro iodo-octanes covalent modification carbon nanotube under UV-irradiation is disclosed.People such as MinooJ.Moghaddam are in " Nano Letters " (" nanometer communication ", 2004,4 phases, the 89-93 page) deliver and be entitled as " Highly efficient binding of DNA on the sidewalls and tips of carbonnanotubes using photochemistry " (" utilizing photochemistry ") efficiently in conjunction with the way of DNA to carbon nanotube tube wall and end, the way with a kind of trinitride covalent modification carbon nanotube under UV-irradiation is disclosed.But these photochemical methods all need special functionalization thing, have limited its application.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of method of photochemical carbon nanotube modifying is provided, make the mixture of carbon nanotube and benzophenone and benzhydrol obtain functionalized carbon nanotube under the irradiation of UV-light, this method is simple, practical, efficient is very high.
The present invention is achieved by the following technical solutions:
The present invention mixes the formation mixing solutions with carbon nanotube and benzophenone, benzhydrol in organic solvent, by the time after benzophenone, the benzhydrol dissolving, mixing solutions is placed on carries out ultrasonication in the ultrasonic wave, then mixing solutions is reacted under UV-irradiation, do not stop simultaneously to stir, the washing reaction product with the remaining product drying in washing back, obtains functionalized carbon nanotube.
Described benzophenone has following structure:
Wherein
Be phenyl ring; C=0 is a carbonyl.
Described benzhydrol has following structure:
Wherein
Be phenyl ring; OH is a hydroxyl.
Described carbon nanotube is single wall or multi-walled carbon nano-tubes, and they are conductor or semi-conductor.
Describedly react under UV-irradiation, the reaction times is 10 minutes to 20 hours.
The mol ratio of described benzophenone and benzhydrol at 1:10 between the 10:1.
Described ultrasonication, ultrasonic 5 to 120 minutes of in ultrasonic wave, carrying out.
Described functionalized carbon nanotube, its functional group is a benzhydrol.
Benzhydrol is with covalent linkage and carbon nanotube bonding on the tube wall of described functionalized carbon nanotube.
The inventive method is simple and practical, and efficient is very high, and thermogravimetric analysis finds that the functional group be grafted to carbon nano tube surface can account for 50% of gross weight, and institute responds and all can carry out under the condition of gentleness, and does not need the experimental installation of complexity.The functionalized carbon nanotube that the present invention obtains can well be dispersed in the organic solvent, can with the convenient reaction of other compounds, and can combine with other polymers and be used for preparing nano composite material.
Embodiment
Below embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Get 5 milligrams of Single Walled Carbon Nanotube, benzophenone 2.5 grams, benzhydrol 2.527 grams, add 20 milliliters of benzene and mix the formation mixing solutions, by the time after benzophenone and the benzhydrol dissolving, mixing solutions is placed in the ultrasonic wave ultrasonic 5 minutes, is placed on then under the UV-light and shines, reacted 2 hours, ceaselessly stir simultaneously, collecting reaction product is washed 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.
Weight analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 42% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Embodiment 2
Get 5 milligrams of Single Walled Carbon Nanotube, benzophenone 2.5 grams, benzhydrol 2.527 grams, add 20 milliliters of benzene and mix the formation mixing solutions, by the time after benzophenone and the benzhydrol dissolving, mixing solutions is placed in the ultrasonic wave ultrasonic 10 minutes, is placed on then under the UV-light and shines, reacted 2 hours, ceaselessly stir simultaneously, collecting reaction product is washed 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.Thermogravimetric analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 50% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Embodiment 3
Get 5 milligrams of Single Walled Carbon Nanotube, benzophenone 2.5 grams, benzhydrol 2.527 grams, add 20 milliliters of benzene and mix the formation mixing solutions, by the time after benzophenone and the benzhydrol dissolving, mixing solutions is placed in the ultrasonic wave ultrasonic 120 minutes, is placed on then under the UV-light and shines, reacted 2 hours, do not stop simultaneously to stir, collecting reaction product is washed 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.Thermogravimetric analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 33% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Embodiment 4
Get 5 milligrams of Single Walled Carbon Nanotube, benzophenone 5 grams, benzhydrol 0.5054 gram, add 10 milliliters of benzene and mix the formation mixing solutions, by the time after benzophenone and the benzhydrol dissolving, mixing solutions is placed in the ultrasonic wave ultrasonic 10 minutes, is placed on then under the UV-light and shines, reacted 10 minutes, do not stop simultaneously to stir, collecting reaction product is washed 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.Thermogravimetric analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 11% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Embodiment 5
Get 5 milligrams of Single Walled Carbon Nanotube, benzophenone 2.5 grams, benzhydrol 25.27 grams, add 30 milliliters of benzene and mix the formation mixing solutions, by the time after benzophenone and the benzhydrol dissolving, mixing solutions is placed in the ultrasonic wave ultrasonic 10 minutes, is placed on then under the UV-light and shines, reacted 20 hours, do not stop simultaneously to stir, collecting reaction product is washed 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.Thermogravimetric analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 6% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Embodiment 6
Get 5 milligrams of multi-walled carbon nano-tubes, benzophenone 2.5 grams, benzhydrol 2.527 grams add 20 milliliters of benzene and mix the formation mixing solutions, after benzophenone and the benzhydrol dissolving by the time, mixing solutions is placed in the ultrasonic wave ultrasonic 10 minutes, be placed on then under the UV-light and shine, reacted 2 hours, do not stop simultaneously to stir, collecting reaction product, wash 2 times with tetrahydrofuran (THF), the remaining product in washing back under vacuum dry 3 hours obtains functionalized carbon nanotube.Thermogravimetric analysis finds that the functional group that is grafted to carbon nano tube surface accounts for 23% of gross weight.Raman spectrum, UV spectrum and infrared spectra show that the benzhydrol functional group of modifying on the carbon nanotube tube wall is connected with covalent linkage and carbon nanotube.
Functionalized carbon nanotube is stable in ethanol, solution not precipitation generation in static 10 days.And functionalized carbon nanotube is unstable in ethanol, in ethanol ultrasonic after, static 1 day whole precipitation just.
Claims (7)
1, a kind of method of photochemical carbon nanotube modifying, it is characterized in that, carbon nanotube and benzophenone, benzhydrol are mixed the formation mixing solutions in organic solvent, by the time after benzophenone, the benzhydrol dissolving, mixing solutions is placed on carries out ultrasonication in the ultrasonic wave, then mixing solutions is reacted under UV-irradiation, do not stop simultaneously to stir, the washing reaction product with the remaining product drying in washing back, obtains functionalized carbon nanotube;
Described organic solvent specifically is meant: benzene.
2, the method for photochemical carbon nanotube modifying according to claim 1 is characterized in that, described carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
3, the method for photochemical carbon nanotube modifying according to claim 1 is characterized in that, the mol ratio of described benzophenone and benzhydrol at 1:10 between the 10:1.
4, the method for photochemical carbon nanotube modifying according to claim 1 is characterized in that, describedly carries out ultrasonication in ultrasonic wave, and ultrasonic time is 5 to 120 minutes.
5, the method for photochemical carbon nanotube modifying according to claim 1 is characterized in that, describedly reacts under UV-irradiation, and the reaction times is 10 minutes to 20 hours.
6, the method for photochemical carbon nanotube modifying according to claim 1 is characterized in that, described functionalized carbon nanotube, and its functional group is a benzhydrol.
According to the method for claim 1 or 6 described photochemical carbon nanotube modifyings, it is characterized in that 7, benzhydrol is with covalent linkage and carbon nanotube bonding on the tube wall of described functionalized carbon nanotube.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101188935A CN100491240C (en) | 2006-11-30 | 2006-11-30 | Photochemical carbon nanotube modifying process |
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| CNB2006101188935A CN100491240C (en) | 2006-11-30 | 2006-11-30 | Photochemical carbon nanotube modifying process |
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| CN1986398A CN1986398A (en) | 2007-06-27 |
| CN100491240C true CN100491240C (en) | 2009-05-27 |
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| CN104861785B (en) * | 2013-12-23 | 2017-11-14 | 北京阿格蕾雅科技发展有限公司 | High dispersive CNT composite conducting ink |
| 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 |
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Granted publication date: 20090527 Termination date: 20111130 |