CN1331741C - Preparation method for water soluble carbon nanotube - Google Patents
Preparation method for water soluble carbon nanotube Download PDFInfo
- Publication number
- CN1331741C CN1331741C CNB2005100186177A CN200510018617A CN1331741C CN 1331741 C CN1331741 C CN 1331741C CN B2005100186177 A CNB2005100186177 A CN B2005100186177A CN 200510018617 A CN200510018617 A CN 200510018617A CN 1331741 C CN1331741 C CN 1331741C
- Authority
- CN
- China
- Prior art keywords
- nanometer tube
- carbon nanometer
- water
- carbon nanotube
- carbon
- 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.)
- Expired - Fee Related
Links
Images
Abstract
The present invention relates to a preparation method for a water-soluble carbon nanometer tube, which is a low damage physical method on the basis of non-covalence surface modification of disazo dye molecules for a carbon nanometer tube so as to realize the high water solubility and the effective separation of the carbon nanometer tube. The method uses azo dyes, the carbon nanometer tube and water as raw materials, and a commercial carbon nanometer tube is washed by water to neutral and is dried after purified; then, the obtain the purification carbon nanometer tube is uniformly mixed with excessive azo dyes, and a conventional physical grinding or ultrasonic dispersion method is used for sufficiently dissolving or dispersing the carbon nanometer tube. The carbon nanometer tube prepared by the present invention has the advantages of good water solubility and high separation rate. Because the azo dyes are used for selectively dissolving the carbon nanometer tube, the method can be used for purifying and separating the carbon nanometer tube, and the azo dyes have the advantages of low cost, stability and good biocompatibility. The method has the advantages of simple technology, mild conditions and easy control of technological parameters, and thus, the large-scale industry application of the water-soluble carbon nanometer tube is greatly promoted.
Description
Technical field
The present invention relates to a kind ofly prepare the method for water-soluble carbon nanometer tube based on the disazo dye molecule non-covalent modification, be applicable to this carbon nanotube dissolving, purifying, separate, derive and follow-up practical application.
Background technology
Since being found in 1991, carbon nanotube is just with its particular structure, electricity, mechanics and optical characteristics and be subjected to numerous investigators' favor in field of nanometer technology potential wide application prospect.Almost each possible practical application all requires carbon nanotube to have good dissolving or dispersing property.Yet industrial extensive synthetic carbon nanotube often contains the various impurity that comprise catalyzer and various decolorizing carbon.And, owing to there is the bigger specific surface that Van der Waals force and carbon nanotube itself are had between extremely strong pipe between the carbon nanotube, the many pencil forms that form side by side with a large amount of single-root carbon nano-tubes of carbon nanotube exist, make carbon nanotube be dissolved in all solvents hardly, this has greatly limited the practical application of carbon nanotube.Therefore, the dissolving of carbon nanotube or dispersion technology are the popular domains of carbon nanotube basis research always.The method that disperses or dissolves of carbon nanotube has two big classes: a class is by various chemical covalent modification methods the sidewall of carbon nanotube or the port behind the open pipe to be carried out covalency to derive, realize that its dissolving disperses or effectively peels off, though this method solubleness is good, the charge stripping efficiency height, but thereby the perfect structure of meeting destroying carbon nanometer tube itself influences its various premium propertiess, and complex disposal process is difficult to control; Another kind of is with various non-covalent modification methods, by polymkeric substance or small molecules aggregate (as surfactant micelle) parcel of carbon nanotube is realized that its dissolving disperses and peels off, these class methods are little to the damage of carbon nanotube, basically keep its original performance, but often have that solubleness is little, poor stability and the low shortcoming of charge stripping efficiency, and some method needs expensive specific synthetic agent.All these unfavorable factors have all greatly limited the large-scale practical application of carbon nanotube.
Summary of the invention
For overcoming these problems that exist in the prior art, make carbon nanotube obtain better application, the invention provides a kind of brand-new preparation method who the non-covalent surface of carbon nanotube is modified the highly water-soluble of realizing carbon nanotube and the carbon nanotube of effectively peeling off based on disazo dye molecule, carbon nanotube with this method preparation not only has the characteristics of the highly water-soluble and the high charge stripping efficiency of covalent modification method, the low damage feature that also has the non-covalent modification method, and this method itself have with low cost, technology simple, be convenient to advantage such as large-scale industrial application.
The technical solution adopted for the present invention to solve the technical problems is: with Congo red, carbon nanotube and water is raw material, as follows preparation:
(1) with ordinary method with commercialization carbon nanotube purifying, be washed with water to neutral and oven dry, obtain purifying carbon nano-tube;
(2), with conventional physical grinding or ultra-sonic dispersion method carbon nanotube is fully dissolved then or disperse with the purifying carbon nano-tube of gained and excessive Congo red mixing;
(3) mixture that obtains is removed the Congo red molecule of excessive free state through washing, get water-soluble carbon nanometer tube.
Aforesaid method is fit to preparation single wall, double-walled and multi-walled carbon nano-tubes.
Owing to can be peeled off into single-root carbon nano-tube effectively with the carbon nano-tube bundle of method for preparing, the good water solubility of carbon nanotube, so for chemical covalent modification method, have low abrasive advantage, and for existing non-covalent method, have better solvability and charge stripping efficiency.Again because of the selective dissolution of azoic dyestuff to carbon nanotube, the purifying that this method also can be used for carbon nanotube with separate, and azoic dyestuff low price, stability and Bc are good.Therefore this water-soluble carbon nanometer tube can be used widely at purifying, dissolving or dispersion, separation and the chemistry of carbon nanotube or physics aspect such as derive., mild condition simple from operation steps preparation technology of the present invention as can be seen, processing parameter are more easy to control, and these favourable conditions will promote greatly that also this water-soluble carbon nanometer tube can be by large-scale industrial application.
Description of drawings
Accompanying drawing is the solubility property comparison diagram of various carbon nanotubes.(a). carbon nanotube+water; (b). carbon nanotube+N, dinethylformamide (DMF); (c). carbon nanotube+Congo red+water; (d). carbon nanotube+Congo red+DMF; (e). it is Congo red (c) to remove free state through washing; (f). the dispersion again in water behind the water-soluble carbon nanometer tube complete drying (e); (g). carbon nanotube+sodium lauryl sulphate (SDS)+water
Embodiment
Embodiment 1
With the commercialization carbon nanotube through 48 hours backflow purifying of the rare nitric acid of 2.6mol/L, be washed with water to neutral and oven dry, again the purifying carbon nano-tube of gained and excessive disazo dyes are mixed back grinding 2 hours, the carbon nanotube of gained and the mixture of azoic dyestuff can be water-soluble fully, and wherein the azoic dyestuff of excessive free state can wash with water and remove and do not reduce the water-soluble of carbon nanotube.
Embodiment 2
With the commercialization carbon nanotube through 48 hours backflow purifying of the rare nitric acid of 2.6mol/L, be washed with water to neutral and oven dry, it is molten in right amount in water that the purifying carbon nano-tube of gained and excessive disazo dyes mix the back, and ultrasonic to there not being solid residue in the high-power ultrasonic instrument, wherein the azoic dyestuff of excessive free state can wash with water and remove and do not reduce the water-soluble of carbon nanotube.
Below in conjunction with the water-soluble carbon nanometer tube of description of drawings non-covalent modification provided by the present invention preparation good solubility property in water.From figure, can be clear that, though 48 hours backflow purification process of the rare nitric acid of process, carbon nanotube still insoluble fully in water (in the accompanying drawing (a)); When with this organic solvent dispersing Nano carbon tubes commonly used of DMF, most carbon nanotubes all settle down, and have only minute quantity to be dissolved in wherein (in the accompanying drawing (b)); Through carbon nanotube then dissolving fully in water of Congo red processing, and solubleness is up to 3.5mg/ml (in the accompanying drawing (c)); But the carbon nanotube of Congo red processing almost insoluble in DMF (in the accompanying drawing (d)); Meanwhile, when excessive free state Congo red after water washing is removed, the solubility property of carbon nanotube influenced hardly (in the accompanying drawing (e)); What is interesting is that no free state is Congo red when existing, thoroughly lost its good water-soluble (in accompanying drawing (f)) after being dissolved in the carbon nanotube complete drying in the water; As a comparison, this anion surfactant of the most widely used sodium lauryl sulphate (SDS) is used to disperse purified carbon nanotube in the world, but the carbon nanotube that still has only minute quantity be dissolved in the water (～0.1mg/ml), its solubleness is well below the prepared water-soluble carbon nanometer tube of the present invention (3.5mg/ml) (in the accompanying drawing (g)).
Claims (1)
1. the preparation method of a water-soluble carbon nanometer tube is characterized in that: with Congo red, carbon nanotube and water is raw material, preparation as follows:
(1) with ordinary method with commercialization carbon nanotube purifying, be washed with water to neutral and oven dry, obtain purifying carbon nano-tube;
(2), with conventional physical grinding or ultra-sonic dispersion method carbon nanotube is fully dissolved then or disperse with the purifying carbon nano-tube of gained and excessive Congo red mixing;
(3) mixture that obtains is removed the Congo red molecule of excessive free state through washing, get water-soluble carbon nanometer tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186177A CN1331741C (en) | 2005-04-27 | 2005-04-27 | Preparation method for water soluble carbon nanotube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186177A CN1331741C (en) | 2005-04-27 | 2005-04-27 | Preparation method for water soluble carbon nanotube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1699155A CN1699155A (en) | 2005-11-23 |
| CN1331741C true CN1331741C (en) | 2007-08-15 |
Family
ID=35475441
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100186177A Expired - Fee Related CN1331741C (en) | 2005-04-27 | 2005-04-27 | Preparation method for water soluble carbon nanotube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1331741C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145885A (en) * | 2011-03-04 | 2011-08-10 | 南京师范大学 | Method for preparing surface phosphorylated water-soluble carbon nanotube and prepared carbon nanotube |
| CN102535198B (en) * | 2011-12-08 | 2014-01-29 | 陕西科技大学 | Dyeing method of acid dyes assisted by functionalized carbon nanotubes |
| CN102516816A (en) * | 2011-12-08 | 2012-06-27 | 陕西科技大学 | Preparation method of acidic dye modified based on carbon nano-tubes, and dyeing method |
| CN110589806B (en) * | 2019-07-25 | 2022-08-05 | 武汉大学 | Efficient purification method of water-dispersible carbon nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436721A (en) * | 2002-02-08 | 2003-08-20 | 中国科学院化学研究所 | Prepn of water soluble carbon nanotube |
| JP2005028560A (en) * | 2003-07-07 | 2005-02-03 | Naotoshi Nakajima | Method for manufacturing water-soluble carbon nanotube using dna and oligonucleotide |
| CN1587031A (en) * | 2004-08-26 | 2005-03-02 | 复旦大学 | Process for preparing surface carboxyl modified carbon nano tube |
-
2005
- 2005-04-27 CN CNB2005100186177A patent/CN1331741C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436721A (en) * | 2002-02-08 | 2003-08-20 | 中国科学院化学研究所 | Prepn of water soluble carbon nanotube |
| JP2005028560A (en) * | 2003-07-07 | 2005-02-03 | Naotoshi Nakajima | Method for manufacturing water-soluble carbon nanotube using dna and oligonucleotide |
| CN1587031A (en) * | 2004-08-26 | 2005-03-02 | 复旦大学 | Process for preparing surface carboxyl modified carbon nano tube |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1699155A (en) | 2005-11-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105253878B (en) | A kind of method that expanded graphite or graphene are directly prepared under normal temperature and pressure | |
| CN1331741C (en) | Preparation method for water soluble carbon nanotube | |
| CN103910354B (en) | Method for preparing graphene through large-scale aqueous phase | |
| CN106185895A (en) | A kind of graphene dispersion liquid and preparation method thereof | |
| CN108550856A (en) | Carbon nano tube/graphene composite conducting slurry and preparation method thereof | |
| CN109095462A (en) | A kind of graphene and its preparation method and application | |
| CN102746236B (en) | Method for preparing functionalized graphene oxide | |
| CN102500318B (en) | Surface modification method of carbon nanotube, carbon nanotube and application thereof | |
| CN103447008A (en) | Three-component cationic dye adsorbent and preparation method thereof | |
| CN105271175B (en) | A kind of process for dispersing of CNT | |
| CN106582994B (en) | A kind of device and production method continuously preparing graphene slurry | |
| CN101746747B (en) | Preparation method of nylon-6 grafting modified carbon nano tubes | |
| CN104211053A (en) | Preparation method of modified graphene aqueous dispersion | |
| CN104307491A (en) | Modified graphene for efficiently adsorbing methyl orange dye and preparation method of modified graphene | |
| CN104386699B (en) | Double-template legal system is for the method for many shells mesoporous silicon oxide nanomaterial | |
| CN103172048A (en) | Preparation method of water-soluble carbon nanotube | |
| CN102553532A (en) | Method for preparing magnetic carbon nano-tube adsorbent having high adsorption capacity and used for removing dye from aqueous phase | |
| CN108676346A (en) | graphene modified aqueous polyurethane and preparation method thereof | |
| JP5629960B2 (en) | Method for producing composite adhesive, composite adhesive and adhesive sheet | |
| CN106564881A (en) | Preparation of reduced graphene oxide by one-step method | |
| CN105645385B (en) | A method of preparing graphene | |
| CN105540567A (en) | Single multi-wall carbon nanotube dispersion liquid and preparation method thereof | |
| CN101941690A (en) | Method for improving dispersibility of single-walled carbon nanotube in aqueous solution | |
| CN102311441A (en) | Production method of sodium copper chlorophyllin | |
| CN110589806B (en) | Efficient purification method of water-dispersible carbon nano material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |