CN101298325A - Low-voltage microwave radiation carbon nanotube hydroxyl modification method - Google Patents
Low-voltage microwave radiation carbon nanotube hydroxyl modification method Download PDFInfo
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- CN101298325A CN101298325A CNA2008100647571A CN200810064757A CN101298325A CN 101298325 A CN101298325 A CN 101298325A CN A2008100647571 A CNA2008100647571 A CN A2008100647571A CN 200810064757 A CN200810064757 A CN 200810064757A CN 101298325 A CN101298325 A CN 101298325A
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Abstract
The invention provides a hydroxy modification method for a low-pressure microwave radiation carbon nanometer tube, it relates to the hydroxy modification method of the carbon nanometer tube and solves the problems of the existing modification technology on nanometer tube that the technical process is complex, the reaction time is long, and the energy consumption and the cost are high. The modification method includes the steps of: 1. soaking carbon nanometer tube into alkali solution, then heat by microwave under low pressure, and remove the upper layer of alkali solution after the cooling and precipitation to obtain the precipitate; 2. cleaning and dry the precipitate to obtain the hydroxy-modified carbon nanometer tube. The invention greatly shortens the reaction time and has the advantages of simple technique, low energy consumption and low cost.
Description
Technical field
The present invention relates to a kind of carbon nanotube hydroxyl modification method.
Background technology
Japan Electronic Speculum expert Iijima has found CNT (carbon nano-tube) first in 1991, because the CNT (carbon nano-tube) mechanical property is strong, tensile strength is big, snappiness good, so be applied in many field of compound material such as electronics, metal, plastics, fiber, pottery widely; CNT (carbon nano-tube) has become best up to now hydrogen storage material, and also can be used as the excellent carrier of multiclass catalysts.But because the wetting ability of carbon nanotube is very poor, if require the performance of maximization performance CNT (carbon nano-tube), to the carbon nano-tube modification link that is absolutely necessary.Though it is at present many to the method for carbon nano-tube modification, the patent that " a kind of preparation method of carbon nano tube surface hydroxyl modification (Chinese application number: 200610025273.7; applying date: on March 30th, 2006, publication number: CN1843904) " wherein comparatively successful arranged; But the shortcoming of this method is a High Temperature High Pressure hydro-thermal method processing carbon nanotube exists complex process, long reaction time, energy consumption to reach the cost height more greatly.
Summary of the invention
The present invention seeks to carbon nanotube is carried out modification to exist complex process, long reaction time, energy consumption to reach the high problem of cost greatly, and a kind of method of low-voltage microwave radiation carbon nanotube hydroxyl modification is provided in order to solve prior art.
A kind of method of low-voltage microwave radiation carbon nanotube hydroxyl modification realizes according to the following steps: one, 0.5～2g carbon nanotube is immersed in the alkaline solution of 50mL, be that 700W, pressure are to react 1～10min under the condition of 0.2～0.5MPa at microwave power then, taking-up is cooled to room temperature, adds distilled water and staticly settles; Two, with throw out with polytetrafluoroethylene film, clean to the pH of the filtrate of dripping be 6～7, dry under 80～105 ℃ condition then, promptly get the carbon nanotube of hydroxyl modification; Wherein alkaline concentration is 1.5～15mol/L in the step 1.
The microwave radiation that the present invention adopts has been strengthened the hydroxyl modification of alkaline solution to carbon nanotube, increases the wetting ability of carbon nanotube, and oxy radical can strengthen its dispersiveness in the aqueous solution, can strengthen it to adsorption of metal ions and ion-exchange capacity simultaneously.It can shorten the reaction times greatly---only for " a kind of preparation method of carbon nano tube surface hydroxyl modification (Chinese application number: 200610025273.7; applying date: on March 30th, 2006; open day: on October 11st, 2006) " 1/24～1/48, enhance productivity, do not have thermograde in the reaction process, reaction is evenly; In this experimental system, carbon nanotube belongs to high loss material, when microwave radiation has shortened the reaction times, has also reduced energy consumption, saves cost.
Description of drawings
The infrared absorpting light spectra of the carbon nanotube hydroxyl that Fig. 1 obtains for embodiment 12.
Embodiment
Embodiment one: a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification method of present embodiment realizes according to the following steps: one, 0.5～2g carbon nanotube is immersed in the alkaline solution of 50mL, be that 700W, pressure are to react 1～10min under the condition of 0.2～0.5MPa at microwave power then, taking-up is cooled to room temperature, adds distilled water and staticly settles; Two, with throw out with polytetrafluoroethylene film, clean to the pH of the filtrate of dripping be 6～7, dry under 80～105 ℃ condition then, promptly get the carbon nanotube of hydroxyl modification; Wherein alkaline concentration is 1.5～15mol/L in the step 1.
Carbon nanotube is a multi-walled carbon nano-tubes in the present embodiment.
Embodiment two: what present embodiment and embodiment one were different is in the step 1 0.8～1.4g carbon nanotube to be immersed in the alkaline solution of 50mL.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is in the step 1 1g carbon nanotube to be immersed in the alkaline solution of 50mL.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different is that alkaline solution is one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide, ammoniacal liquor, yellow soda ash in the step 1.Other step and parameter are identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is that pressure is 0.3～0.4MPa in the step 1.Other step and parameter are identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is that pressure is 0.35MPa in the step 1.Other step and parameter are identical with embodiment one.
Embodiment seven: present embodiment and embodiment one are different be in the step 1 heat-up time be 3～7min.Other step and parameter are identical with embodiment one.
Embodiment eight: present embodiment and embodiment one are different be in the step 1 heat-up time be 5min.Other step and parameter are identical with embodiment one.
Embodiment nine: present embodiment and embodiment one are different is that the aperture of polytetrafluoroethylene film in the step 2 is 0.20 μ m.Other step and parameter are identical with embodiment one.
Embodiment ten: what present embodiment and embodiment one were different is that drying temperature is 90～100 ℃ in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 11: what present embodiment and embodiment one were different is that drying temperature is 95 ℃ in the step 2.Other step and parameter are identical with embodiment one.
Embodiment 12: present embodiment low-voltage microwave radiation carbon nanotube hydroxyl modification method realizes according to the following steps: one, the 1g carbon nanotube is immersed in the sodium hydroxide reactor of 50mL, be that 700W, pressure are under the condition of 0.2MPa at microwave power then, reaction 5min, taking-up is cooled to room temperature, add distilled water and staticly settle the sodium hydroxide solution that the upper strata is removed in the back, get throw out; Two, with throw out with the aperture be 0.20 μ m polytetrafluoroethylene film, water circulating pump suction filtration clean to the pH of the filtrate of dripping be 7, then under 105 ℃ condition, dry 24h promptly gets the carbon nanotube of hydroxyl modification; Wherein alkaline concentration is 1.5mol/L in the step 1.
The hydroxyl carbon nanotube of gained modification in the present embodiment is 3400cm in wave number by the infrared absorption spectrum of Fig. 1 as can be seen
-1About the OH absorption peak is arranged, the carbon nanotube cochain that also just can draw hydroxyl modification has OH, modification success.
The hydroxyl carbon nanotube of gained modification in the present embodiment and unmodified carbon nanotube adopt the phenolic waste water of microwave reinforced AOP technical finesse 6000mg/L as catalyzer, as can be seen from Table 1, the hydroxyl carbon nanotube Pyrogentisinic Acid's of modification treatment effect is better than not carrying out modified carbon nanotube, and the clearance of phenol is greatly improved.
| Treatment process | Phenol clearance (%) |
| Unmodified carbon nanotube is handled phenol | 50.0 |
| The hydroxylation carbon nanotube is handled phenol | 63.2 |
Table 1
Claims (7)
1, a kind of method of low-voltage microwave radiation carbon nanotube hydroxyl modification, it is characterized in that the low-voltage microwave radiation carbon nanotube hydroxyl modification method realizes according to the following steps: one, 0.5～2g carbon nanotube is immersed in the alkaline solution of 50mL, be that 700W, pressure are to react 1～10min under the condition of 0.2～0.5MPa at microwave power then, taking-up is cooled to room temperature, adds distilled water and staticly settles; Two, with throw out with polytetrafluoroethylene film, clean to the pH of the filtrate of dripping be 6～7, dry under 80～105 ℃ condition then, promptly get the carbon nanotube of hydroxyl modification; Wherein alkaline concentration is 1.5～15mol/L in the step 1.
2, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1 is characterized in that in the step 1 1g carbon nanotube being immersed in the alkaline solution of 50mL.
3, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1 is characterized in that in step 1 alkaline solution is one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide, ammoniacal liquor, yellow soda ash.
4, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1 is characterized in that pressure is 0.3～0.4MPa in the step 1.
5, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1 is characterized in that be 3～7min heat-up time in the step 1.
6, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1, the aperture that it is characterized in that polytetrafluoroethylene film in the step 2 are 0.20 μ m.
7, the method for a kind of low-voltage microwave radiation carbon nanotube hydroxyl modification according to claim 1 is characterized in that drying temperature is 90～100 ℃ in the step 2.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105057001A (en) * | 2015-07-22 | 2015-11-18 | 上海应用技术学院 | Modified multi-walled carbon nanotube loaded iron-based catalyst and preparation method and application thereof |
| CN106698395A (en) * | 2016-12-06 | 2017-05-24 | 袁洁 | Modified carbon nanotube for solar energy |
| CN109487363A (en) * | 2018-11-30 | 2019-03-19 | 山传雷 | A kind of multifunctional carbon nanotube plant source fiber and preparation method thereof |
| CN109505028A (en) * | 2018-11-30 | 2019-03-22 | 山传雷 | A kind of long-acting broad-spectrum antibacterial day tea fiber and preparation method thereof |
| CN110357090A (en) * | 2019-07-19 | 2019-10-22 | 广东工业大学 | A kind of preparation method of the Nano diamond hydrosol |
-
2008
- 2008-06-18 CN CN2008100647571A patent/CN101298325B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105057001A (en) * | 2015-07-22 | 2015-11-18 | 上海应用技术学院 | Modified multi-walled carbon nanotube loaded iron-based catalyst and preparation method and application thereof |
| CN106698395A (en) * | 2016-12-06 | 2017-05-24 | 袁洁 | Modified carbon nanotube for solar energy |
| CN109487363A (en) * | 2018-11-30 | 2019-03-19 | 山传雷 | A kind of multifunctional carbon nanotube plant source fiber and preparation method thereof |
| CN109505028A (en) * | 2018-11-30 | 2019-03-22 | 山传雷 | A kind of long-acting broad-spectrum antibacterial day tea fiber and preparation method thereof |
| CN109487363B (en) * | 2018-11-30 | 2021-06-08 | 青岛邦特生态纺织科技有限公司 | Multifunctional carbon nanotube plant source fiber and preparation method thereof |
| CN110357090A (en) * | 2019-07-19 | 2019-10-22 | 广东工业大学 | A kind of preparation method of the Nano diamond hydrosol |
| CN110357090B (en) * | 2019-07-19 | 2020-12-29 | 广东工业大学 | Preparation method of nano-diamond hydrosol |
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