CN103043650A - Modified CNT (carbon nano tube) - Google Patents
Modified CNT (carbon nano tube) Download PDFInfo
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- CN103043650A CN103043650A CN2012105943258A CN201210594325A CN103043650A CN 103043650 A CN103043650 A CN 103043650A CN 2012105943258 A CN2012105943258 A CN 2012105943258A CN 201210594325 A CN201210594325 A CN 201210594325A CN 103043650 A CN103043650 A CN 103043650A
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- carbon nano
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- carbon nanotube
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Abstract
The invention provides a modified CNT. The composition comprises components as follows: a multi-walled CNT, ethanediamine, thionyl chloride, concentrated nitric acids, tetrahydrofuran, distilled water and absolute ethyl alcohol. The invention further provides a composite method for the modified CNT to obtain the CNT with excellent performance, and the CNT is an ideal reinforcement body for composite materials.
Description
Technical field
The present invention relates to chemical field, particularly a kind of modified carbon nano-tube.
Background technology
The ideal that carbon nanotube is considered to matrix material strengthens body, can improve the toughness of matrix material, and intensity and electroconductibility etc. have great researching value.But, because specific surface area and the surface energy of carbon nanotube are larger, so that carbon nanotube is easy to reunite, affected the dispersion of carbon nanotube in matrix.And carbon nano tube surface is smooth, is nonpolar, is insoluble to general organic solvent, and is all incompatible with all polymkeric substance, so that the interface interaction of matrix material is not strong.
In order to improve the dispersion of carbon nanotube in polymkeric substance and the interface binding power of enhancing carbon nanotube and polymeric matrix, must carry out surface treatment to carbon nanotube.
Summary of the invention
The present invention proposes a kind of modified carbon nano-tube, has solved the dispersion of carbon nanotube in polymkeric substance and the interface binding power problem of carbon nanotube and polymeric matrix in the prior art.
Technical scheme of the present invention is achieved in that modified carbon nano-tube, contains following material: multi-walled carbon nano-tubes, quadrol, sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol.
The invention has the beneficial effects as follows:
(1) the present invention has obtained a kind of modified carbon nano-tube, has solved the scattering problem of carbon nanotube in polymkeric substance.
(2) the present invention has obtained a kind of modified carbon nano-tube, has solved the interface binding power problem of carbon nanotube and polymeric matrix.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, the below will do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art, apparently, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the production technological process of modified carbon nano-tube of the present invention.
Embodiment
The present invention is through extensive and deep research, by adopting mixing acid cutting multi-walled carbon nano-tubes, make its be with-COOH and-the OH group, carry out again on this basis the modification of grafting quadrol, thereby finish the present invention.Fig. 1 is the production technological process of modified carbon nano-tube of the present invention, the step 10 nitration mixture (vitriol oil: concentrated nitric acid=3: 1) multi-walled carbon nano-tubes is carried out the acid cutting; The sour cutting carbon nanotubes of step 20 and sulfur oxychloride reaction make the carboxyl of carbon nano tube surface be converted into acyl chlorides; Step 30 is got quantitative quadrol and carbon pipe, and 2: 1 ratio is carried out graft reaction to the carbon pipe; Behind step 40 graft reaction, obtain modified carbon nano-tube.
Multi-walled carbon nano-tubes
The unique texture of carbon nanotube has determined that it has many special physics and chemistry character.The C=C covalent linkage that forms carbon nanotube is the most stable chemical bond of nature, so that carbon nanotube has very excellent mechanical property.The mechanical property of carbon nanotube and little diameter thereof and large length-to-diameter ratio will be brought better reinforced effects to carbon nano tube compound material.
The multi-walled carbon nano-tubes that the present invention uses has adopted the CVD method to produce.
Preferably, described multi-walled carbon nano-tubes mean diameter is less than 8nm, length 10~30m, and purity is greater than 95% (by rare nitric acid purifying).
Quadrol
1,2-diaminoethane.The molecular structure skeleton symbol is H
2NCH
2CH
2NH
2Water white thick liquid has the smell of ammonia.Water-soluble and ethanol is slightly soluble in ether.Quadrol is highly basic, meets easily salify of acid; Generate hydrate when water-soluble; Energy absorbs airborne moisture and carbonic acid gas generates nonvolatile carbonate.Quadrol can form complex compound with many inorganic salt.
Preferably, described quadrol prepares by dichloroethane law, and reaction equation is:
ClCH
2CH
2Cl+2NH
4OH→HCl·H
2NCH
2CH
2NH
2·HCl+2H
2O[2NaOH]→NH
2CH
2CH
2NH
2+2Nacl
Other components: sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol is marketable material.
Below in conjunction with specific embodiment, further set forth the present invention.The experimental technique of unreceipted actual conditions in the following example is measured according to national standard usually.If there is not corresponding national standard, then carry out according to general international standard, normal condition or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage, and described polymericular weight is number-average molecular weight.
Unless otherwise defined or explanation, same meanings of being familiar with of all specialties used herein and scientific words and those skilled in the art.Any method similar or impartial to described content and material all can be applicable in the inventive method in addition.
Building-up process is as follows:
Take by weighing the original multi-walled carbon nano-tubes of 5g (p-MWNTs), place the nitration mixture (vitriol oil: concentrated nitric acid=3: 1) 50 ℃ of backflow 4h of 300ml, then vacuum filtration, the black solid that obtains is filtered with distilled water flushing repeatedly, until filtrate pH value near neutrality till, obtain sour cutting carbon nanotubes (a-MWNTs), the product that obtains is placed 80 ℃ of dry 24h of vacuum drying oven, obtain the modified carbon nano-tube after acid is cut; Carbon nanotube after the acid cutting and sulfur oxychloride are reacted backflow 24h, the carboxyl of carbon nano tube surface is converted to acyl chlorides.After washing the dechlorination sulfoxide with tetrahydrofuran (THF) afterwards, vacuum-drying 24h under room temperature.Measure an amount of quadrol and carbon pipe, behind 130-140 ℃ of back flow reaction 24h, be cooled to room temperature in 2: 1 ratios.Reaction product is leached the rear washing with alcohol of using dry, obtain the function modified carbon nanotube of quadrol (MWNTs-EDA).
The solvability contrast of the multi-walled carbon nano-tubes of modification and common multi-walled carbon nano-tubes: original carbon nanotube is because specific surface area is large, easily reunite, and surface group seldom, be difficult in solvent, dissolve, carbon nanotube after the modification since with-OH and-COOH isoreactivity group, increase so that modified carbon nano-tube is active, can be dissolved in the partial solvent.
By thermogravimetic analysis (TGA), show that the more original carbon nanotube of ethylene diamine-modified carbon nanotube resistance toheat descends, the grafting molecule begins to come off about 220 ℃, and the massfraction of grafting is about 15%.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a modified carbon nano-tube is characterized in that, comprising: contain following component: carbon nanotube, quadrol, sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol.
2. modified carbon nano-tube according to claim 1 is characterized in that, described carbon nanotube is multi-walled carbon nano-tubes, caliber: 10-30nm, purity>90%.
3. modified carbon nano-tube according to claim 2 is characterized in that, described multi-walled carbon nano-tubes is the multi-walled carbon nano-tubes of mixed acid cutting, and it is with carboxyl and hydroxyl.
4. modified carbon nano-tube according to claim 3 is characterized in that, described multi-walled carbon nano-tubes and quadrol grafting become a kind of carbon nanotube that is modified.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103872282A (en) * | 2014-03-31 | 2014-06-18 | 河南理工大学 | Polymer lithium ion battery diaphragm and preparation method thereof |
CN104261385A (en) * | 2014-09-25 | 2015-01-07 | 鄂尔多斯市君实科技有限责任公司 | Modified carbon material as well as preparation method and application thereof |
CN105440510A (en) * | 2015-12-10 | 2016-03-30 | 青岛海特新蓝生物科技有限公司 | Inlet manifold of engine |
CN105464859A (en) * | 2015-12-10 | 2016-04-06 | 青岛海特新蓝生物科技有限公司 | Intake manifold with modified carbon nano tubes |
CN105552502A (en) * | 2015-12-29 | 2016-05-04 | 青岛玻莱莫斯新材料技术有限公司 | Carbon nano multilayer balun |
CN105569888A (en) * | 2015-12-10 | 2016-05-11 | 青岛海特新蓝生物科技有限公司 | Engine gas intake manifold adopting modified carbon nanotube |
CN106025304A (en) * | 2016-06-29 | 2016-10-12 | 王尧尧 | Preparation method and application of Pt/PdAu/CNT-ZnO2 methanol fuel battery catalyst |
CN116333499A (en) * | 2023-02-28 | 2023-06-27 | 南京航空航天大学 | Wave-absorbing low-shrinkage methyl vinyl silicone rubber and preparation method thereof |
-
2012
- 2012-12-10 CN CN2012105943258A patent/CN103043650A/en active Pending
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103872282A (en) * | 2014-03-31 | 2014-06-18 | 河南理工大学 | Polymer lithium ion battery diaphragm and preparation method thereof |
CN103872282B (en) * | 2014-03-31 | 2016-04-13 | 河南理工大学 | A kind of polymer lithium cell diaphragm and preparation method thereof |
CN104261385A (en) * | 2014-09-25 | 2015-01-07 | 鄂尔多斯市君实科技有限责任公司 | Modified carbon material as well as preparation method and application thereof |
CN104261385B (en) * | 2014-09-25 | 2016-09-07 | 鄂尔多斯市君实科技有限责任公司 | A kind of modified carbonaceous components and its preparation method and application |
CN105440510A (en) * | 2015-12-10 | 2016-03-30 | 青岛海特新蓝生物科技有限公司 | Inlet manifold of engine |
CN105464859A (en) * | 2015-12-10 | 2016-04-06 | 青岛海特新蓝生物科技有限公司 | Intake manifold with modified carbon nano tubes |
CN105569888A (en) * | 2015-12-10 | 2016-05-11 | 青岛海特新蓝生物科技有限公司 | Engine gas intake manifold adopting modified carbon nanotube |
CN105552502A (en) * | 2015-12-29 | 2016-05-04 | 青岛玻莱莫斯新材料技术有限公司 | Carbon nano multilayer balun |
CN106025304A (en) * | 2016-06-29 | 2016-10-12 | 王尧尧 | Preparation method and application of Pt/PdAu/CNT-ZnO2 methanol fuel battery catalyst |
CN116333499A (en) * | 2023-02-28 | 2023-06-27 | 南京航空航天大学 | Wave-absorbing low-shrinkage methyl vinyl silicone rubber and preparation method thereof |
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Application publication date: 20130417 |