CN101049926A - Method for dispersing Nano carbon tubes - Google Patents
Method for dispersing Nano carbon tubes Download PDFInfo
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- CN101049926A CN101049926A CN 200710068641 CN200710068641A CN101049926A CN 101049926 A CN101049926 A CN 101049926A CN 200710068641 CN200710068641 CN 200710068641 CN 200710068641 A CN200710068641 A CN 200710068641A CN 101049926 A CN101049926 A CN 101049926A
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- carbon nanotube
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910021392 nanocarbon Inorganic materials 0.000 title claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 37
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims description 14
- 239000013543 active substance Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000006396 nitration reaction Methods 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 230000011218 segmentation Effects 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 229960003964 deoxycholic acid Drugs 0.000 claims description 3
- KXGVEGMKQFWNSR-LLQZFEROSA-N deoxycholic acid Chemical compound C([C@H]1CC2)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)[C@@H](O)C1 KXGVEGMKQFWNSR-LLQZFEROSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000001728 nano-filtration Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000004108 freeze drying Methods 0.000 abstract description 2
- 150000007513 acids Chemical class 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000002525 ultrasonication Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
This invention discloses a freeze-drying method for dispersing carbon nanotubes. The method comprises: treating carbon nanotubes by ultrasonication in mixed acids or surfactant to obtain stable dispersion in water, adding carbon nanotube dispersion into a freeze drier, quenching to -40 deg.C, keeping for 1-2 h, vacuumizing until the pressure in the drying chamber is below 100 Pa, drying 8-16 h, heating in stages to room temperature, and drying for 1-10 h in each temperature stage to obtain well dispersed loose sponge-like carbon nanotube powder. The method has easy operation, and the treated carbon nanotubes have obviously improved dispersibility, thus can be used to prepare composite.
Description
Technical field
The present invention relates to the method for dispersing Nano carbon tubes.
Background technology
Carbon nanotube (CNTs) is a kind of important nano material because its particular structure and performance, at present CNT (carbon nano-tube) be used as one independently Application Areas studied.Carbon nanotube becomes the monodimension nanometer material that has application potential with its high length-to-diameter ratio and superpower mechanical property, and it is used and has related to many aspects such as nano-device and matrix material.But when carbon nanotube was used as the wild phase of superpolymer and metallic matrix, the intensity of material did not significantly improve, and this mainly is because the carbon pipe is difficult to homodisperse in matrix, formed bigger coacervate easily.Therefore managing to improve the carbon pipe gets dispersing property and has great science and using value.
Make the method for carbon nanotube stable dispersion in different liquid phase mediums existing multiple, all can make stable suspersion among the carbon Guan Zaishui as nitration mixture (vitriol oil and concentrated nitric acid) supersound process, tensio-active agent (as Sodium dodecylbenzene sulfonate) etc., thereby improve the dispersiveness of carbon pipe in liquid phase, but after this dispersed system process usual way drying, reunion between the carbon nanotube significantly strengthens on the contrary, is difficult to carry out actual application.Therefore, explore a kind of method of simple possible carbon nanotube is disperseed, make it easy to use, still have very big challenge.
Summary of the invention
The method that the purpose of this invention is to provide a kind of dispersing Nano carbon tubes.
The method of dispersing Nano carbon tubes of the present invention, employing be freeze-drying, its step is as follows:
1) adopts the processing of nitration mixture supersound process or tensio-active agent that carbon nanotube is dispersed in and become steady suspension in the water, said nitration mixture supersound process is to be in 3: 1 the mixing solutions with the volume ratio that carbon nanotube is immersed in the vitriol oil and concentrated nitric acid, sonic oscillation was handled 8～12 hours, centrifugation or filter out carbon nanotube then with nanofiltration membrane, equal 7 with deionized water wash to pH value, immersing the deionized water for ultrasonic vibration again becomes steady suspension; It is carbon nanotube to be immersed in stir in the tensio-active agent or sonic oscillation becomes steady suspension that said tensio-active agent is handled;
2) suspension liquid of carbon nanotube is put into freeze drier, is chilled to-40 ℃ and be incubated 1～2 hour, then vacuum pumping chamber to kiln air pressure less than 100Pa, dry 8～16 hours;
3) the chamber vacuum tightness that keeps dry is constant, segmentation progressively elevated temperature until room temperature, and when arriving every section temperature value dry 1-10 hour.
In the step 3) of the present invention, said segmentation temperature can be set arbitrarily in-40 ℃～25 ℃ scopes, but must be in the dry sufficiently long time below 0 ℃, to guarantee that the moisture in the sample is fully got rid of.Generally getting segmentation temperature-30 ℃ ,-20 ℃ ,-10 ℃, 0 ℃, 10 ℃, 25 ℃ is advisable.
Among the present invention, said tensio-active agent can be Sodium dodecylbenzene sulfonate or sodium deoxycholate.
Beneficial effect of the present invention is:
Working method is simple, and the dispersiveness of the carbon nanotube of handling through the present invention significantly improves, and has created condition for carbon nanotube really is applied to prepare composite.
Description of drawings
Fig. 1 is the photo of dispersing Nano carbon tubes of the present invention: (a) photo of macroscopical accumulation body; (b) transmission electron microscope photo.
Embodiment
Embodiment 1:
1) at room temperature the 1g carbon nanotube is immersed in the mixed acid solution that is made into by the 90ml vitriol oil and 30ml concentrated nitric acid, sonic oscillation was handled 8 hours, centrifugation goes out carbon nanotube then, with the carbon nanotube that obtains repeatedly with deionized water wash, pH value up to washings equals 7, immerse 100ml deionized water for ultrasonic vibration 30 minutes again, make carbon nanotube dispersion suspension in water;
2) above suspension is put into freeze drier, be chilled to-40 ℃, and-40 ℃ of insulations 1 hour; Open vacuum system, kiln air pressure is reduced to below the 100Pa, dry 10 hours;
3) keep dry that to be lower than 100Pa constant for chamber vacuum tightness, be warmed up to-30 ℃, dry 8 hours; Be warmed up to-20 ℃, dry 5 hours; Be warmed up to-10 ℃, dry 4 hours; Be warmed up to 0 ℃, dry 3 hours; Be warmed up to 10 ℃, dry 1 hour; Be warmed up to 25 ℃, dry 1 hour.Close vacuum system, open the freeze drier intake valve, take out sample, disperseed, fluffy spongy carbon nanotube powder (see figure 1).
Embodiment 2:
1) under the room temperature 1g sodium deoxycholate is dissolved in the 100ml deionized water, the 1g carbon nanotube is joined in this solution, stir half an hour, obtain stable carbon nano tube suspension;
2) above suspension is put into freeze drier, be chilled to-40 ℃, and-40 ℃ of insulations 1 hour.Open vacuum system, kiln air pressure is reduced to below the 100Pa, dry 14 hours;
3) keep dry that to be lower than 100Pa constant for chamber vacuum tightness, be warmed up to-30 ℃, dry 10 hours; Be warmed up to-20 ℃, dry 8 hours; Be warmed up to-10 ℃, dry 6 hours; Be warmed up to 0 ℃, dry 5 hours; Be warmed up to 10 ℃, dry 2 hours; Be warmed up to 25 ℃, dry 1 hour.Close vacuum system, open the freeze drier intake valve, take out sample, disperseed, fluffy spongy carbon nanotube powder.
Embodiment 3:
1) under the room temperature 0.5g Sodium dodecylbenzene sulfonate is dissolved in the 100ml deionized water, the 1g carbon nanotube is joined in this solution, stir half an hour, obtain stable carbon nano tube suspension,
2) above suspension is put into freeze drier, be chilled to-40 ℃, and-40 ℃ of insulations 2 hours.Open vacuum system, kiln air pressure is reduced to below the 100Pa, dry 8 hours,
3) keep dry that to be lower than 100Pa constant for chamber vacuum tightness, be warmed up to-30 ℃, dry 6 hours; Be warmed up to-20 ℃, dry 5 hours; Be warmed up to-10 ℃, dry 3 hours; Be warmed up to 0 ℃, dry 2 hours; Be warmed up to 10 ℃, dry 1 hour; Be warmed up to 25 ℃, dry 1 hour.Close vacuum system, open the freeze drier intake valve, take out sample, disperseed, fluffy spongy carbon nanotube powder.
Claims (3)
1. the method for a dispersing Nano carbon tubes, its step is as follows:
1) adopts the processing of nitration mixture supersound process or tensio-active agent that carbon nanotube is dispersed in and become steady suspension in the water, said nitration mixture supersound process is to be in 3: 1 the mixing solutions with the volume ratio that carbon nanotube is immersed in the vitriol oil and concentrated nitric acid, sonic oscillation was handled 8～12 hours, centrifugation or filter out carbon nanotube then with nanofiltration membrane, equal 7 with deionized water wash to pH value, immersing the deionized water for ultrasonic vibration again becomes steady suspension; It is carbon nanotube to be immersed in stir in the tensio-active agent or sonic oscillation becomes steady suspension that said tensio-active agent is handled;
2) suspension liquid of carbon nanotube is put into freeze drier, is chilled to-40 ℃ and be incubated 1～2 hour, then vacuum pumping chamber to kiln air pressure less than 100Pa, dry 8～16 hours;
3) the chamber vacuum tightness that keeps dry is constant, segmentation progressively elevated temperature until room temperature, and when arriving every section temperature value dry 1-10 hour.
2. the method for dispersing Nano carbon tubes according to claim 1 is characterized in that the said segmentation temperature of step 3) is-30 ℃ ,-20 ℃ ,-10 ℃, 0 ℃, 10 ℃, 25 ℃.
3. the method for dispersing Nano carbon tubes according to claim 1 is characterized in that said tensio-active agent is Sodium dodecylbenzene sulfonate or sodium deoxycholate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710068641 CN101049926A (en) | 2007-05-15 | 2007-05-15 | Method for dispersing Nano carbon tubes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710068641 CN101049926A (en) | 2007-05-15 | 2007-05-15 | Method for dispersing Nano carbon tubes |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417795B (en) * | 2008-11-24 | 2010-11-17 | 山东大学 | Method for preparing carbonaceous nano tube viscoelastic fluid |
| CN102218143A (en) * | 2011-06-10 | 2011-10-19 | 郑州大学 | Water dispersion type carbon nano-tube freeze-dried powder and preparation method thereof |
| CN102275899A (en) * | 2010-06-11 | 2011-12-14 | 南京宏德纳米材料有限公司 | Preparation of amphiprotic carbon nanotube dispersed powder |
| CN102557032A (en) * | 2012-03-09 | 2012-07-11 | 桂林理工大学 | Preparation method of high-purity silicon carbide nano fibers |
| CN102936008A (en) * | 2012-11-27 | 2013-02-20 | 东风汽车有限公司 | Honeycomb carbon nano tube macroscopic body and preparation method thereof |
| CN103350993A (en) * | 2013-04-26 | 2013-10-16 | 南京大学 | Method for chemical modification of carbon nano-tubes |
| CN104418316A (en) * | 2013-08-27 | 2015-03-18 | 清华大学 | Carbon nanotube sponge body and preparation method thereof |
| WO2015096590A1 (en) * | 2013-12-23 | 2015-07-02 | 北京阿格蕾雅科技发展有限公司 | Method for improving single-wall carbon nanotube dispersion |
| CN105329873A (en) * | 2014-07-08 | 2016-02-17 | 清华大学 | Carbon nanotube sponge and preparation method thereof |
| CN105439112A (en) * | 2015-12-02 | 2016-03-30 | 南昌大学 | Method for improving dispersity of carbon nano calabash structure material in ethanol water solution |
| CN105906832A (en) * | 2016-06-29 | 2016-08-31 | 德阳烯碳科技有限公司 | Preparation method of graphene-containing water-based electrothermal film |
| CN107010614A (en) * | 2017-04-24 | 2017-08-04 | 苏州纳磐新材料科技有限公司 | Aqueous liquid dispersion of carbon nanomaterial and preparation method thereof |
| CN109761223A (en) * | 2017-11-09 | 2019-05-17 | 北京华碳元芯电子科技有限责任公司 | The method for removing carbon nano-tube film surface organic dispersing agent |
| CN110894068A (en) * | 2018-11-12 | 2020-03-20 | 江苏天奈科技股份有限公司 | Preparation method of easily-dispersible carbon nanotube powder and carbon nanotube powder |
| CN111559742A (en) * | 2019-12-25 | 2020-08-21 | 江西悦安新材料股份有限公司 | Method for improving stability of carbon nano tube |
| CN113563785A (en) * | 2021-07-12 | 2021-10-29 | 安徽桑瑞斯环保新材料有限公司 | Graphene epoxy based anticorrosion base powder and preparation method thereof |
| CN113912987A (en) * | 2021-10-21 | 2022-01-11 | 浙江工业大学 | Modified carbon nanotube toughened epoxy resin composite material and preparation method thereof |
-
2007
- 2007-05-15 CN CN 200710068641 patent/CN101049926A/en active Pending
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417795B (en) * | 2008-11-24 | 2010-11-17 | 山东大学 | Method for preparing carbonaceous nano tube viscoelastic fluid |
| CN102275899A (en) * | 2010-06-11 | 2011-12-14 | 南京宏德纳米材料有限公司 | Preparation of amphiprotic carbon nanotube dispersed powder |
| CN102218143A (en) * | 2011-06-10 | 2011-10-19 | 郑州大学 | Water dispersion type carbon nano-tube freeze-dried powder and preparation method thereof |
| CN102218143B (en) * | 2011-06-10 | 2012-08-15 | 郑州大学 | Water dispersion type carbon nano-tube freeze-dried powder and preparation method thereof |
| CN102557032A (en) * | 2012-03-09 | 2012-07-11 | 桂林理工大学 | Preparation method of high-purity silicon carbide nano fibers |
| CN102936008B (en) * | 2012-11-27 | 2016-03-16 | 东风汽车公司 | A kind of cellular carbon nano-tube macroscopic body and preparation method thereof |
| CN102936008A (en) * | 2012-11-27 | 2013-02-20 | 东风汽车有限公司 | Honeycomb carbon nano tube macroscopic body and preparation method thereof |
| CN103350993A (en) * | 2013-04-26 | 2013-10-16 | 南京大学 | Method for chemical modification of carbon nano-tubes |
| CN104418316A (en) * | 2013-08-27 | 2015-03-18 | 清华大学 | Carbon nanotube sponge body and preparation method thereof |
| CN104418316B (en) * | 2013-08-27 | 2017-01-25 | 清华大学 | Carbon nanotube sponge body and preparation method thereof |
| US9738795B2 (en) | 2013-12-23 | 2017-08-22 | Beijing Aglaia Technology Development Co., Ltd. | Method for improving single-wall carbon nanotube dispersion |
| WO2015096590A1 (en) * | 2013-12-23 | 2015-07-02 | 北京阿格蕾雅科技发展有限公司 | Method for improving single-wall carbon nanotube dispersion |
| CN105329873A (en) * | 2014-07-08 | 2016-02-17 | 清华大学 | Carbon nanotube sponge and preparation method thereof |
| CN105329873B (en) * | 2014-07-08 | 2018-02-27 | 清华大学 | CNT sponge and preparation method thereof |
| CN105439112A (en) * | 2015-12-02 | 2016-03-30 | 南昌大学 | Method for improving dispersity of carbon nano calabash structure material in ethanol water solution |
| CN105906832B (en) * | 2016-06-29 | 2019-07-26 | 德阳烯碳科技有限公司 | A kind of preparation method of graphene water-based electric heating film |
| CN105906832A (en) * | 2016-06-29 | 2016-08-31 | 德阳烯碳科技有限公司 | Preparation method of graphene-containing water-based electrothermal film |
| CN107010614A (en) * | 2017-04-24 | 2017-08-04 | 苏州纳磐新材料科技有限公司 | Aqueous liquid dispersion of carbon nanomaterial and preparation method thereof |
| CN109761223A (en) * | 2017-11-09 | 2019-05-17 | 北京华碳元芯电子科技有限责任公司 | The method for removing carbon nano-tube film surface organic dispersing agent |
| CN110894068A (en) * | 2018-11-12 | 2020-03-20 | 江苏天奈科技股份有限公司 | Preparation method of easily-dispersible carbon nanotube powder and carbon nanotube powder |
| CN111559742A (en) * | 2019-12-25 | 2020-08-21 | 江西悦安新材料股份有限公司 | Method for improving stability of carbon nano tube |
| CN113563785A (en) * | 2021-07-12 | 2021-10-29 | 安徽桑瑞斯环保新材料有限公司 | Graphene epoxy based anticorrosion base powder and preparation method thereof |
| CN113912987A (en) * | 2021-10-21 | 2022-01-11 | 浙江工业大学 | Modified carbon nanotube toughened epoxy resin composite material and preparation method thereof |
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