CN1843904A - Method for conducting modification of surface hydroxy group of carbon nanotube - Google Patents
Method for conducting modification of surface hydroxy group of carbon nanotube Download PDFInfo
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Abstract
The invention relates to a method for conducting modification of surface hydroxy group of carbon nanotube which comprises subjecting the carbon nanotubes to high temperature and high pressure thermal treatment under alkaline conditions.
Description
Technical field
The invention belongs to technical field of inorganic material, be specifically related to a kind of preparation method of carbon nanotube of conducting modification of surface hydroxy group.
Technical background
Carbon nanotube is the nano level coaxial clyinder of the seamless hollow that is rolled into of the graphite by laminated structure, cylindrical two ends respectively have one " cap " that formed by half soccerballene spheroid molecule, generally can divide for the Single Walled Carbon Nanotube be made up of one deck graphite and by two kinds of the coaxial multi-walled carbon nano-tubes of forming of multilayer graphite.
Because the distinctive immanent structure of carbon nanotube (length-to-diameter ratio, chirality etc.), carbon nanotube shows peculiar physics and chemical property, is a kind of type material that catches people's attention.Can be used for preparing field emission device, nano electron device and one dimension gan nanometer rod.Carbon nanotube is a kind of potential hydrogen storage material, and is one of mechanical property best material since the dawn of human civilization, has very big using value aspect polymer blending.But because carbon nanotube has huge molecular weight, directly caused the insolubility of carbon nanotube, thereby limited the application of carbon nanotube in a lot of fields.Therefore, the preparation of soluble carbon nanotube becomes a difficult problem of being badly in need of solution, also becomes the popular direction of scientists study.In the preparation process of soluble carbon nanotube, the carbon nanotube of carboxyl surface modification occupies an important position, and a lot of preparation process all are through carboxy-modified process.Then study seldom for the hydroxyl that is reactive group equally.
With regard to the carbon nano tube surface hydroxyl modification, present bibliographical information seldom mainly adopts ozonize, then through hydroboration reduction, perhaps solid mechanical means.The common issue with that these two kinds of method reactions all exist is to have technical difficulty aspect the relatively large modified carbon nano-tube.
Summary of the invention
The objective of the invention is to obtain a kind of simple, good reproducibility, can mass-produced surface hydroxylation modified carbon nano-tube the preparation method.
The preparation method of the conducting modification of surface hydroxy group carbon nanotube that the present invention proposes is that a kind of high temperature high pressure process that adopts under alkaline condition obtains the method for conducting modification of surface hydroxy group carbon nanotube.The surface hydroxyl controllable number, output is big.And in the whole process, shortening carbon nano-tube not.
The preparation method of a kind of carbon nano tube surface hydroxyl modification that the present invention proposes, under alkaline condition, adopt High Temperature High Pressure hydro-thermal method that carbon nanotube is carried out surface modification, obtain the carbon nanotube of conducting modification of surface hydroxy group, by changing the concentration of basic solution, hydroxy radical content that can the controlling carbon nanotube surface.
Concrete grammar of the present invention is as follows:
Carbon nanotube is added in the inorganic alkaline aqueous solution for preparing, and the weight ratio of carbon nanotube and alkaline aqueous solution is 0.001～0.1, and the concentration of alkaline aqueous solution is 0.1-5.0M, stir the back and move into reactor, after the sealing, react 2～8h down at 150～300 ℃, the reaction postcooling is to room temperature, filtering with microporous membrane is isolated the carbon nanotube of hydroxyl modification, and with deionized water wash 3～5 times, last, put into vacuum drying oven, 30～50 ℃ of dryings promptly obtain the carbon nanotube of conducting modification of surface hydroxy group.
Among the present invention, used carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
Among the present invention, the concentration of alkaline aqueous solution is 1.0-3.0M.
Among the present invention, used mineral alkali is one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, cesium hydroxide, ammoniacal liquor, yellow soda ash, the salt of wormwood.
Among the present invention, used alkali is preferably potassium hydroxide or sodium hydroxide.
Among the present invention, be 22-26 hour time of drying preferably in vacuum drying oven.
The inventive method raw material is easy to get, and preparation process is simple, good reproducibility, and output is big.Concentration by the control basic solution makes the carbon nanotube hydroxyl controllable number of the conducting modification of surface hydroxy group that makes, and carbon nanotube keeps original length, not by brachymemma.
Embodiment
Embodiment 1:2.0g multi-wall carbon nano-tube pipe powder adds in the potassium hydroxide aqueous solution of 50mL0.1M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 150 ℃, stop heating behind the reaction 8h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 3 times, 30 ℃ of dry 22h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Embodiment 2:2.0g Single Walled Carbon Nanotube powder adds in the potassium hydroxide aqueous solution of 50mL5M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 300 ℃, stop heating behind the reaction 2h, reduce to room temperature.Isolate the Single Walled Carbon Nanotube of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 5 times, 50 ℃ of dry 26h of vacuum drying oven obtain the Single Walled Carbon Nanotube of conducting modification of surface hydroxy group.
Embodiment 3:0.5g multi-wall carbon nano-tube pipe powder adds in the potassium hydroxide aqueous solution of 50mL0.5M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 200 ℃, stop heating behind the reaction 6h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 45 ℃ of dry 24h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Embodiment 4:2.0g multi-wall carbon nano-tube pipe powder adds in the aqueous sodium carbonate of 50mL1.5M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 200 ℃, stop heating behind the reaction 6h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 45 ℃ of dry 24h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Embodiment 5:1.0g Single Walled Carbon Nanotube powder adds in the ammonia soln of 50mL2M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 250 ℃, stop heating behind the reaction 6.5h, reduce to room temperature.Isolate the Single Walled Carbon Nanotube of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 5 times, 45 ℃ of dry 24h of vacuum drying oven obtain the Single Walled Carbon Nanotube of conducting modification of surface hydroxy group.
Embodiment 6:3.0g multi-wall carbon nano-tube pipe powder adds in the wet chemical of 50mL1M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 250 ℃, stop heating behind the reaction 6h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 40 ℃ of dry 24h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Embodiment 7:2.8g multi-wall carbon nano-tube pipe powder adds in the ammonia soln of 50mL5M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 250 ℃, stop heating behind the reaction 6h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 40 ℃ of dry 24h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Embodiment 8:3.0g Single Walled Carbon Nanotube powder adds in the baryta water of 50mL3M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 250 ℃, stop heating behind the reaction 6h, reduce to room temperature.Isolate the Single Walled Carbon Nanotube of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 35 ℃ of dry 26h of vacuum drying oven obtain the Single Walled Carbon Nanotube of conducting modification of surface hydroxy group.
Embodiment 9:4.0g multi-wall carbon nano-tube pipe powder adds in the sodium hydroxide solution of 50mL5M, behind the stirring 5min, move into the stainless steel autoclave (polytetrafluoroethyllining lining is arranged in the still) of 50mL, after the sealing, be warming up to 200 ℃, stop heating behind the reaction 7h, reduce to room temperature.Isolate the multi-walled carbon nano-tubes of hydroxyl modification with 0.45um poly(vinylidene fluoride) filtering with microporous membrane, and with deionized water wash 4 times, 45 ℃ of dry 24h of vacuum drying oven obtain the multi-walled carbon nano-tubes of conducting modification of surface hydroxy group.
Claims (7)
1, a kind of preparation method of carbon nano tube surface hydroxyl modification, it is characterized in that adopting under the alkaline condition High Temperature High Pressure hydro-thermal method that carbon nanotube is carried out surface modification, obtain the carbon nanotube of conducting modification of surface hydroxy group, by changing the concentration of basic solution, hydroxy radical content that can the controlling carbon nanotube surface.
2, the preparation method of carbon nano tube surface hydroxyl modification according to claim 1 is characterized in that concrete grammar is as follows:
Carbon nanotube is added in the alkaline aqueous solution for preparing, and the weight ratio of the carbon nanotube and the inorganic alkaline aqueous solution is 0.001～0.1, and the concentration of alkaline aqueous solution is 0.1-5.0M, stir the back and move into reactor, after the sealing, react 2～8h down at 150～300 ℃, the reaction postcooling is to room temperature, filtering with microporous membrane is isolated the carbon nanotube of hydroxyl modification, and with deionized water wash 3～5 times, last, put into vacuum drying oven, 30～50 ℃ of dryings promptly obtain the carbon nanotube of conducting modification of surface hydroxy group.
3, the preparation method of the carbon nanotube of conducting modification of surface hydroxy group according to claim 2 is characterized in that used carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
4, the preparation method of the carbon nanotube of conducting modification of surface hydroxy group according to claim 2, the concentration that it is characterized in that alkaline aqueous solution is 1.0-3.0M.
5, the preparation method of the carbon nanotube of conducting modification of surface hydroxy group according to claim 2 is characterized in that used mineral alkali is one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, cesium hydroxide, ammoniacal liquor, yellow soda ash, the salt of wormwood.
6, the preparation method of the carbon nanotube of conducting modification of surface hydroxy group according to claim 5 is characterized in that used mineral alkali is potassium hydroxide or sodium hydroxide.
7, the preparation method of the carbon nanotube of conducting modification of surface hydroxy group according to claim 2 is characterized in that in vacuum drying oven dry 22-26 hour.
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