CN103043650A - Modified CNT (carbon nano tube) - Google Patents

Modified CNT (carbon nano tube) Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
carbon nano
modified
tubes
carbon nanotube
cnt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2012105943258A
Other languages
Chinese (zh)
Inventor
张勇
朱春林
郑典君
王莉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
QINGDAO BAOLIMAN POLYMER MATERIAL RESEARCH INSTITUTE Co Ltd
Original Assignee
QINGDAO BAOLIMAN POLYMER MATERIAL RESEARCH INSTITUTE Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by QINGDAO BAOLIMAN POLYMER MATERIAL RESEARCH INSTITUTE Co Ltd filed Critical QINGDAO BAOLIMAN POLYMER MATERIAL RESEARCH INSTITUTE Co Ltd
Priority to CN2012105943258A priority Critical patent/CN103043650A/en
Publication of CN103043650A publication Critical patent/CN103043650A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Carbon And Carbon Compounds (AREA)

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

A kind of modified carbon nano-tube
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.
CN2012105943258A 2012-12-10 2012-12-10 Modified CNT (carbon nano tube) Pending CN103043650A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2012105943258A CN103043650A (en) 2012-12-10 2012-12-10 Modified CNT (carbon nano tube)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2012105943258A CN103043650A (en) 2012-12-10 2012-12-10 Modified CNT (carbon nano tube)

Publications (1)

Publication Number Publication Date
CN103043650A true CN103043650A (en) 2013-04-17

Family

ID=48056543

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2012105943258A Pending CN103043650A (en) 2012-12-10 2012-12-10 Modified CNT (carbon nano tube)

Country Status (1)

Country Link
CN (1) CN103043650A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
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
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

Cited By (10)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN103043650A (en) Modified CNT (carbon nano tube)
Guo et al. Carbon nanotube-grafted chitosan and its adsorption capacity for phenol in aqueous solution
Jung et al. Phosphate adsorption ability of biochar/Mg–Al assembled nanocomposites prepared by aluminum-electrode based electro-assisted modification method with MgCl2 as electrolyte
Chen et al. Poly (acrylic acid) grafted multiwall carbon nanotubes by plasma techniques for Co (II) removal from aqueous solution
CN102140145B (en) Method for grafting carbon nanotubes by using cyclodextrin
Hegde et al. Functional porous Ce-UiO-66 MOF@ Keratin composites for the efficient adsorption of trypan blue dye from wastewater: A step towards practical implementations
Alimohammady et al. A new modified MWCNTs with 3-aminopyrazole as a nanoadsorbent for Cd (II) removal from aqueous solutions
CN106492761A (en) A kind of preparation method of magnetic hydrogel microsphere
CN106268546A (en) The preparation method of novel environment friendly Graphene hybrid aerogel
CN103881138B (en) A kind of Guanidine Sulfamate 99 fire retardant modification grafting carbon nanotube and preparation method thereof
CN103881137A (en) Melamine flame retardant graft modified carbon nanotube and manufacturing method thereof
CN102093700A (en) Method for preparing graphene/waterborne polyurethane conductive composite material
CN102992374A (en) Preparation method of calcium carbonate micro-spheres
Ge et al. Immobilization of Hg (II) on high-salinity Spirulina residue-induced biochar from aqueous solutions: Sorption and transformation mechanisms by the dual-mode isotherms
CN104495779A (en) Simple and efficient method for preparing three-dimensional carbon nanotubes/graphene hybrid material
CN104261385A (en) Modified carbon material as well as preparation method and application thereof
Teow et al. Synthesis and characterization of graphene shell composite from oil palm frond juice for the treatment of dye-containing wastewater
CN104118895A (en) Method for preparing homogenous nano vaterite type calcium carbonate through limestone acidolysis
AboDalam et al. Rice wastes for green production and sustainable nanomaterials: an overview
Lee et al. Using nanobubblized carbon dioxide for effective microextraction of heavy metals
KR102294440B1 (en) Graphene oxide-carbon nanotube composite, manufacturing method for the same and cement paste comprising the same
Yu et al. Inhibition of organosilane/ATP@ HQ self-healing passivator for pyrite oxidation
CN106433603A (en) Carbon nano-tube doped fracturing fluid system
CN108676346A (en) graphene modified aqueous polyurethane and preparation method thereof
CN105524426B (en) A kind of non-isocyanate polyurethane carbon nano-tube modification epoxy resin composite material and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20130417