CN103626152B - Modification method of carbon nano tube - Google Patents
Modification method of carbon nano tube Download PDFInfo
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- CN103626152B CN103626152B CN201310613933.3A CN201310613933A CN103626152B CN 103626152 B CN103626152 B CN 103626152B CN 201310613933 A CN201310613933 A CN 201310613933A CN 103626152 B CN103626152 B CN 103626152B
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- carbon nanotube
- hydrogen peroxide
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Abstract
The invention discloses a modification method of a carbon nano tube. The method comprises the following steps: mixing anhydrous ethanol with hydrogen peroxide to obtain anhydrous ethanol-hydrogen peroxide liquor; putting pyrrole in the anhydrous ethanol-hydrogen peroxide liquor to obtain anhydrous ethanol-hydrogen peroxide-pyrrole mixed liquor; then, putting the carbon nano tube in the anhydrous ethanol-hydrogen peroxide-pyrrole mixed liquor; carrying out ultrasonic treatment on a mixture formed by anhydrous ethanol-hydrogen peroxide-pyrrole-carbon nano tube; and then, centrifugally separating the carbon nano tube at high speed, cleaning and carrying out ultrasonic treatment, and drying to constant weight to obtain the modified carbon nano tube. The modified carbon nano tube provided by the invention has excellent dispersibility and stability in water and organic solvents, so that treatment of the carbon nano tube at high temperature by commonly using mixed acid is avoided. The modification method has the characteristics of no pollution, good dispersing effect and the like, is simple to operate, and can be used for treating multi-walled and single-wall carbon nano tubes.
Description
Technical field
The present invention relates to field of fine chemical, particularly relate to a kind of method of modifying of carbon nanotube.
Background technology
Carbon nanotube has the performance of a series of excellences such as high mechanics, electricity, optics and calorifics.The application prospect of carbon nanotube in manufacture, microelectronic device, electrode materials, storage hydrogen and support of the catalyst etc. is very extensive, and Application Areas comprises all trades and professions such as electric power, automobile, the energy, chemical industry, environment, biology, machinery, nuclear power.
Because the diameter of carbon nanotube is generally between several to dozens of nanometers, the thickness of tube wall is only several nanometer, there is great specific surface area and surface energy, therefore, carbon nanotube is easy to reunite, and have impact on the uniformly dispersed of it and stability, causes the consistency between the matrix material of institute's modification poor, even carbon nanotube is disperseed in the composite, very necessary to its surface modification.
Conventional method of modifying mainly contains physical modified method and chemic modified method, and physical modified method comprises polymer overmold and the method such as surfactant-modified; Chemic modified method comprises the methods such as mechanochemical modification method, high-energy modification, local chemical modification.
Conventional physical modification method has the shortcomings such as complicated operation, as needs high temperature, high-energy, sometimes also needs complicated equipment; And chemical modification method generally adopts strong acid mixed solution to carry out preoxidation, and then carry out the chemical processing of scion grafting.Use nitration mixture process easily to produce poisonous, harmful gas, contaminate environment, and need higher temperature of reaction, operational difficulty.Technique is simple, with low cost, the surface modification of carbon nanotube process of environmental protection is developing direction from now on.
Summary of the invention
Based on this, be necessary to provide the method for modifying of the carbon nanotube of simple and the dispersed and good stability of a kind for the treatment of process.
A method of modifying for carbon nanotube, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide being 20 ~ 30wt% by dehydrated alcohol and concentration mixes, and obtains dehydrated alcohol-hydrogen peroxide mixed solution, the weight ratio of described dehydrated alcohol and hydrogen peroxide is 1:0.5 ~ 5; Pyrroles is put into described dehydrated alcohol-hydrogen peroxide mixed solution, obtain dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, the weight ratio of described pyrroles and dehydrated alcohol-hydrogen peroxide mixed solution is 0.1 ~ 5:100; Carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions again, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture, the weight ratio of described carbon nanotube and dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions is 0.1 ~ 10:100; Dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is carried out supersound process, and then high speed centrifugation isolates carbon nanotube;
(2) cleaning of carbon nanotube is with dry: carried out cleaning and centrifuging treatment by the carbon nanotube that step (1) obtains, then dry to constant weight, to obtain final product.
Wherein in an embodiment, the pyrroles described in step (1) and the weight ratio of dehydrated alcohol-hydrogen peroxide mixed solution are 0.5 ~ 3:100.
Wherein in an embodiment, the weight ratio of the carbon nanotube described in step (1) and dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions is 0.5 ~ 5:100.
Wherein in an embodiment, the frequency of the supersound process described in step (1) is 22 ~ 100kHz, and power is 100 ~ 2000W.
Wherein in an embodiment, the sonication treatment time described in step (1) is 1 ~ 3h.
Wherein in an embodiment, the cleaning described in step (2) and the number of times of centrifuging treatment are 4 ~ 6 times.
Wherein in an embodiment, the bake out temperature described in step (2) is 50 ~ 100 DEG C.
Wherein in an embodiment, step (2) described cleaning time use solution be ethanol and deionized water mixing solutions, described ethanol is identical with the weight ratio of hydrogen peroxide with the dehydrated alcohol described in step (1) with the weight ratio of deionized water.
In the method for modifying of the carbon nanotube that the present invention relates to, the carbon nanotube through pyrroles's modification avoids conventional nitration mixture pyroprocessing carbon nanotube, has the features such as simple to operate, pollution-free, safety and environmental protection, dispersion effect are good; And the carbon nanotube through pyrroles's modification has excellent dispersiveness and stability in water and organic solvent; Meanwhile, present invention employs aliquots of deionized water and replace hydrogen peroxide cleaning, advantage is that the modified surface structure avoiding processed carbon nanotube is destroyed; The pyrroles's method of modifying that the present invention relates to can process many walls and Single Walled Carbon Nanotube.
Accompanying drawing explanation
The carbon nanotube that Fig. 1 is through pyrroles's modification places the photomacrograph after 20 days in water.
Photomacrograph after the carbon nanotube that Fig. 2 is through pyrroles's modification places 20 days in weight ratio is the dimethylbenzene of 1:1 and alcohol mixed solvent.
The carbon nanotube that Fig. 3 is through pyrroles's modification places the photomacrograph after 20 days in ethanol.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Embodiment 1
The method of modifying of the carbon nanotube described in the present embodiment, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide mixing by 50g dehydrated alcohol and 50g concentration being 30wt%, obtains dehydrated alcohol-hydrogen peroxide mixed solution; 0.1g pyrroles is put into above-mentioned 100g dehydrated alcohol-hydrogen peroxide mixed solution, form dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions; Again 4g carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture; Again by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in Ultrasonic Cleaners, in 28kHz, 100W ultrasound environments, 2.5h is processed under normal temperature condition, then by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in supercentrifuge, be isolate carbon nanotube under the condition of 16000rpm at rotating speed;
(2) cleaning of carbon nanotube is with dry: the dehydrated alcohol-deionized water carbon nanotube that obtains of cleaning step (1) repeatedly then by weight ratio being 1:1, then carbon nanotube is inserted in supercentrifuge after cleaning, be isolate carbon nanotube under the condition of 16000rpm at rotating speed, cleaning-centrifugation totally 6 times, carbon nanotube after cleaning-separation is put into baking oven, dry under 80 DEG C of conditions to constant weight, to obtain final product.
In water, the macro morphology after 20 days is placed as shown in Figure 1 through the carbon nanotube of the present embodiment modification, not there is Precipitation in carbon nanotube, by contrast, through conventional nitration mixture pre-treatment, and then with silane coupler modified carbon nanotube, after placing 24h, namely there is partly precipitated.
Known by contrasting, the carbon nanotube obtained by the method for modifying of carbon nanotube described in the present embodiment has excellent dispersiveness and stability in water.
Embodiment 2
The method of modifying of the carbon nanotube described in the present embodiment, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide mixing by 100g dehydrated alcohol and 400g concentration being 20wt%, obtains dehydrated alcohol-hydrogen peroxide mixed solution; 15g pyrroles is put into above-mentioned 500g dehydrated alcohol-hydrogen peroxide mixed solution, form dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions; Again 0.515g carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture; Again by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in Ultrasonic Cleaners, in 80kHz, 500W ultrasound environments, 3h is processed under normal temperature condition, then by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in supercentrifuge, be isolate carbon nanotube under the condition of 16000rpm at rotating speed;
(2) cleaning of carbon nanotube is with dry: the dehydrated alcohol-deionized water carbon nanotube that obtains of cleaning step (1) repeatedly then by weight ratio being 1:4, then carbon nanotube is inserted in supercentrifuge after cleaning, be isolate carbon nanotube under the condition of 16000rpm at rotating speed, cleaning-centrifugation totally 5 times, carbon nanotube after cleaning-separation is put into baking oven, dry under 70 DEG C of conditions to constant weight, to obtain final product.
Through the carbon nanotube dispersed of the present embodiment modification in weight ratio is the dimethylbenzene of 1:1 and the mixed solvent of ethanol, place after 20 days, as shown in Figure 2, solution presents uniform black, does not have Precipitation.By contrast, through conventional nitration mixture pre-treatment, and then with silane coupler modified carbon nanotube, after placing 24h, namely there is partly precipitated.
The carbon nanotube obtained by the process of contrast prior art is known, and the carbon nanotube obtained by the method for modifying of carbon nanotube described in the present embodiment has excellent dispersiveness and stability in water.
Embodiment 3
The method of modifying of the carbon nanotube described in the present embodiment, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide mixing by 100g dehydrated alcohol and 300g concentration being 30wt%, obtains dehydrated alcohol-hydrogen peroxide mixed solution; 2g pyrroles is put into above-mentioned 400g dehydrated alcohol-hydrogen peroxide mixed solution, form dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions; Again 2.01g carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture; Again by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in Ultrasonic Cleaners, in 80kHz, 1000W ultrasound environments, 1.5h is processed under normal temperature condition, then by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in supercentrifuge, be isolate carbon nanotube under the condition of 16000rpm at rotating speed;
(2) cleaning of carbon nanotube is with dry: the dehydrated alcohol-deionized water carbon nanotube that obtains of cleaning step (1) repeatedly then by weight ratio being 1:3, then carbon nanotube is inserted in supercentrifuge after cleaning, be isolate carbon nanotube under the condition of 16000rpm at rotating speed, cleaning-centrifugation totally 4 times, carbon nanotube after cleaning-separation is put into baking oven, dry under 50 DEG C of conditions to constant weight, to obtain final product.
Through the carbon nanotube dispersed of the present embodiment modification in dehydrated alcohol, place after 20 days, as shown in Figure 3, solution presents uniform black, does not have Precipitation.By contrast, through conventional nitration mixture pre-treatment, and then with silane coupler modified carbon nanotube, after placing 18h, namely there is partly precipitated
The carbon nanotube obtained by the process of contrast prior art is known, and the carbon nanotube obtained by the method for modifying of carbon nanotube described in the present embodiment has excellent dispersiveness and stability in water.
Embodiment 4
The method of modifying of the carbon nanotube described in the present embodiment, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide mixing by 200g dehydrated alcohol and 100g concentration being 30wt%, obtains dehydrated alcohol-hydrogen peroxide mixed solution; 12g pyrroles is put into above-mentioned 300g dehydrated alcohol-hydrogen peroxide mixed solution, form dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions; Again 15.6g carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture; Again by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in Ultrasonic Cleaners, in 100kHz, 2000W ultrasound environments, 1h is processed under normal temperature condition, then by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in supercentrifuge, be isolate carbon nanotube under the condition of 16000rpm at rotating speed;
(2) cleaning of carbon nanotube is with dry: the dehydrated alcohol-deionized water carbon nanotube that obtains of cleaning step (1) repeatedly then by weight ratio being 2:1, then carbon nanotube is inserted in supercentrifuge after cleaning, be isolate carbon nanotube under the condition of 16000rpm at rotating speed, cleaning-centrifugation totally 6 times, carbon nanotube after cleaning-separation is put into baking oven, dry under 65 DEG C of conditions to constant weight, to obtain final product.
Through the carbon nanotube dispersed of the present embodiment modification be that in the dehydrated alcohol-aqueous solution of 1:2, place after 20 days, solution presents uniform black, does not have Precipitation, and carbon nanotube has excellent dispersiveness and stability in weight ratio.By contrast, through conventional nitration mixture pre-treatment, and then with silane coupler modified carbon nanotube, after placing 20h, namely there is partly precipitated
The carbon nanotube obtained by the process of contrast prior art is known, and the carbon nanotube obtained by the method for modifying of carbon nanotube described in the present embodiment has excellent dispersiveness and stability in water.
Embodiment 5
The method of modifying of the carbon nanotube described in the present embodiment, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide mixing by 40g dehydrated alcohol and 200g concentration being 25wt%, obtains dehydrated alcohol-hydrogen peroxide mixed solution; 12g pyrroles is put into above-mentioned 240g dehydrated alcohol-hydrogen peroxide mixed solution, form dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions; Again 25.2g carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture; Again by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in Ultrasonic Cleaners, in 22kHz, 1500W ultrasound environments, 3h is processed under normal temperature condition, then by dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is inserted in supercentrifuge, be isolate carbon nanotube under the condition of 16000rpm at rotating speed;
(2) cleaning of carbon nanotube is with dry: the dehydrated alcohol-deionized water carbon nanotube that obtains of cleaning step (1) repeatedly then by weight ratio being 1:5, then carbon nanotube is inserted in supercentrifuge after cleaning, be isolate carbon nanotube under the condition of 16000rpm at rotating speed, cleaning-centrifugation totally 5 times, carbon nanotube after cleaning-separation is put into baking oven, dry under 100 DEG C of conditions to constant weight, to obtain final product.
Above-mentioned carbon nanotube dispersed is in water, and place after 20 days, solution presents uniform black, does not have Precipitation, by contrast, through conventional nitration mixture pre-treatment, and then with silane coupler modified carbon nanotube, namely occurs partly precipitated after placing 24h.
The carbon nanotube obtained by the process of contrast prior art is known, and carbon nanotube has excellent dispersiveness and stability in water.
The present invention relates to the method for modifying of carbon nanotube, obtain the carbon nanotube of modification and be uniformly dispersed and excellent in stability in water and organic solvent, technique is simple, be easy to control.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1. a method of modifying for carbon nanotube, is characterized in that, comprises the steps:
(1) surface modification treatment of carbon nanotube: the hydrogen peroxide being 20 ~ 30wt% by dehydrated alcohol and concentration mixes, and obtains dehydrated alcohol-hydrogen peroxide mixed solution, the weight ratio of described dehydrated alcohol and hydrogen peroxide is 1:0.5 ~ 5; Pyrroles is put into described dehydrated alcohol-hydrogen peroxide mixed solution, obtain dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions, the weight ratio of described pyrroles and dehydrated alcohol-hydrogen peroxide mixed solution is 0.1 ~ 5:100; Carbon nanotube is put into dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions again, form dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture, the weight ratio of described carbon nanotube and dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions is 0.1 ~ 10:100; Dehydrated alcohol-hydrogen peroxide-pyrroles-carbon nanotube mixture is carried out supersound process, and high speed centrifugation isolates carbon nanotube, and the frequency of described supersound process is 22 ~ 100kHz, and power is 100 ~ 2000W;
(2) cleaning of carbon nanotube is with dry: carried out cleaning and centrifuging treatment by the carbon nanotube that step (1) obtains, then dry to constant weight, to obtain final product.
2. the method for modifying of carbon nanotube according to claim 1, it is characterized in that, the pyrroles described in step (1) and the weight ratio of dehydrated alcohol-hydrogen peroxide mixed solution are 0.5 ~ 3:100.
3. the method for modifying of carbon nanotube according to claim 1, it is characterized in that, the weight ratio of the carbon nanotube described in step (1) and dehydrated alcohol-hydrogen peroxide-pyrroles's mixing solutions is 0.5 ~ 5:100.
4. the method for modifying of carbon nanotube according to claim 1, is characterized in that, the sonication treatment time described in step (1) is 1 ~ 3h.
5. the method for modifying of carbon nanotube according to claim 1, it is characterized in that, the cleaning described in step (2) and the number of times of centrifuging treatment are 4 ~ 6 times.
6. the method for modifying of carbon nanotube according to claim 1, it is characterized in that, the bake out temperature described in step (2) is 50 ~ 100 DEG C.
7. the method for modifying of carbon nanotube according to claim 1, it is characterized in that, step (2) described cleaning time use solution be ethanol and deionized water mixing solutions, described ethanol is identical with the weight ratio of hydrogen peroxide with the dehydrated alcohol described in step (1) with the weight ratio of deionized water.
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Address after: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee after: ELECTRIC POWER RESEARCH INSTITUTE, GUANGDONG POWER GRID CO., LTD. Patentee after: Institute of metal research, Chinese Academy of Sciences Address before: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee before: Electrical Power Research Institute of Guangdong Power Grid Corporation Patentee before: Institute of metal research, Chinese Academy of Sciences |