CN102557011A - Method for performing functionalization treatment to surface of multi-walled carbon nanotube by utilizing hydrogen peroxide - Google Patents
Method for performing functionalization treatment to surface of multi-walled carbon nanotube by utilizing hydrogen peroxide Download PDFInfo
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- CN102557011A CN102557011A CN2012100624720A CN201210062472A CN102557011A CN 102557011 A CN102557011 A CN 102557011A CN 2012100624720 A CN2012100624720 A CN 2012100624720A CN 201210062472 A CN201210062472 A CN 201210062472A CN 102557011 A CN102557011 A CN 102557011A
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Abstract
The invention discloses a method for performing functionalization treatment to the surface of a multi-walled carbon nanotube by utilizing hydrogen peroxide. The method comprises the following steps of: immersing the multi-walled carbon nanotube into hydrogen peroxide solution, adopting a high-shearing dispersing emulsion machine to produce powerful shearing, material collision and centrifugal extrusion through a rotor rotating at high speed and a precise stator working cavity, strengthening interaction of hydrogen peroxide and the multi-walled carbon nanotube to form a hydroxide radical or a carboxyl and other hydrophilic groups on the surface of the multi-walled carbon nanotube, so that the multi-walled carbon nanotube can be dissolved into ethanol. For the method, strong oxidizers such as nitric acid or additives such as a surface active agent are not needed, hydrophilic functionalization treatment to the surface of the multi-walled carbon nanotube can be realized; the process is simple, environment-friendly, and has low cost; moreover, the effect of using the surface active agent or other hydrophilic macromolecule decoration on the compounding of the carbon nanotube and a resin matrix is avoided, so that the method creates a condition for wide application of the carbon nanotube.
Description
Technical field
The present invention relates to a kind of method of utilizing ydrogen peroxide 50 to carry out the surface-functionalized processing of multi-walled carbon nano-tubes.
Background technology
Carbon nanotube has excellent mechanics, electricity and thermal property, is the desirable toughener of preparation matrix material.But because carbon nano tube surface is unreactiveness, shortage reactive group, thereby the solubleness in all kinds of SOLVENTS is all very low; In addition, because carbon nanotube big L/D ratio and high-specific surface area, under the Van der Waals force effect, very easily reunite and twines, caused carbon nanotube in all kinds of SOLVENTS, all to be difficult to dispersion, limited its application in a lot of fields.
The solvability of carbon nanotube in each kind solvent depends on the surface property of carbon nanotube, so the surface treatment method of carbon nanotube becomes its deliquescent key of restriction.Common carbon nano tube surface treatment process mainly is divided into two types at present, i.e. covalent functionalization and non-covalent functionalization.The covalent functionalization method is through oxygenant and carbon nano tube surface generation chemical reactions such as high density nitric acid, forms hydrophilic radicals such as hydroxyl or carboxyl, improves the solvability of carbon nanotube in water.But the structure of the sp2 that this process can destroying carbon nanometer tube functionalization site influences its electric property and mechanical property, though and oxygenant such as nitric acid still be difficult to thorough removal through repeatedly cleaning, the application of carbon nanotube is caused adverse influence.Non-covalent functionalization method is to adopt tensio-active agent, hydrophilic macromolecule or biomacromolecule etc. carbon nano-tube modified, makes it to possess water-wet behavior.Though this method can farthest keep the integrity of carbon nanotube structure; But the tensio-active agent, high molecular polymer or the biomacromolecule that are difficult to remove have fully been introduced; Not only can influence carbon nanotube and combine, also can influence the electricity of carbon nanotube reinforced composite, hot transport performance simultaneously with interface between the body material.Outside last method, solvent-induced method also is a kind of method of dispersing Nano carbon tubes, but the common toxicity of its solvent for use is big, boiling point is high, and the dispersion efficiency of this method is lower.Therefore; All there is tangible problem in carbon nano tube surface treatment process commonly used at present, and more satisfactory surface treatment method should be the covalent functionalization processing of carbon nanotube being carried out appropriateness, can not influence its electricity and mechanical property; The simultaneous oxidation agent can remove again easily, does not influence environment.
The present invention proposes a kind of method of utilizing ydrogen peroxide 50 to carry out the surface-functionalized processing of multi-walled carbon nano-tubes, it is characterized in that stirring by brute force improving contacting of hydrogen peroxide solution and multi-walled carbon nano-tubes hydrophobic surface, strengthens both interactions.Specific practice is: multi-walled carbon nano-tubes is immersed in the hydrogen peroxide solution; Adopt high-shearing dispersion emulsifying machine; Utilize the rotor of high speed rotating to cooperate the powerful liquid shear of generation, material collision and centrifugal extruding with accurate stator working chamber; Strengthen the interaction of ydrogen peroxide 50 and multi-walled carbon nano-tubes, make the multi-wall carbon nano-tube tube-surface form hydrophilic radicals such as hydroxyl or carboxyl, enable to be dissolved in the ethanol.This method technology is simple, and cost is low, and the functionalization multi-walled carbon nano-tubes of preparation solubleness in ethanol is high; Oxidant hydrogen peroxide and multi-walled carbon nano-tubes level of response are gentle, and residual ydrogen peroxide 50 can remove through methods such as heating easily, can not produce a large amount of cleaning sullages, thereby genus Green Chemistry treatment process.This method is not also appeared in the newspapers at present.
Summary of the invention
The purpose of this invention is to provide a kind of environmental protection and multi-wall carbon nano-tube tube-surface covalent functionalization treatment process cheaply.
Concrete steps are:
(1) multi-walled carbon nano-tubes is heated to 100-200 ℃, kept 3-20 hour, to remove partial impurities and moisture content;
(2) the preparation mass percent concentration is the hydrogen peroxide solution 300ml of 1%-30%, adds the multi-walled carbon nano-tubes after 1g step (1) is handled, and handles 5-120 minute with dispersion emulsifying machine; In 60-90 ℃ loft drier, dry, in the evaporation hydrogen peroxide solution, remove ydrogen peroxide 50 residual in the multi-walled carbon nano-tubes, the wetting ability multi-walled carbon nano-tubes after finally obtaining handling;
When (3) using the multi-walled carbon nano-tubes 100mg after step (2) processing is joined in the 20ml ethanol, sonic oscillation 1-5 minute, promptly obtain the carbon nanotube alcohol dispersion liquid.
Characteristics of the present invention:
(1) only carry out the multi-walled carbon nano-tubes surface treatment with hydrogen peroxide solution, level of response is moderate, can not influence the electricity and the mechanical property of multi-walled carbon nano-tubes; And operating process is simple, and oxygenant removes conveniently, need not cleaning operation, does not pollute the environment;
(2) stir by brute force and improve contacting of hydrogen peroxide solution and multi-walled carbon nano-tubes hydrophobic surface, strengthen both interactions;
(3) present method does not have specific requirement to the diameter of multi-walled carbon nano-tubes;
(4) can directly obtain in ethanol, to have the multi-walled carbon nano-tubes powder of polymolecularity after handling.
Technology of the present invention is simple, cost is low, belongs to green chemistry process, is convenient to realize production application.
Embodiment
Embodiment:
(1) commercial multi-walled carbon nano-tubes (diameter 20-40nm) is heated to 180 ℃, is incubated 5 hours, to remove partial impurities and moisture content;
(2) the preparation mass percent concentration is 6% hydrogen peroxide solution 300ml, adds the multi-walled carbon nano-tubes after 1g step (1) is handled, and handles 30 minutes with the laboratory dispersion emulsifying machine; In 75 ℃ loft drier, dry, in the evaporation hydrogen peroxide solution, remove ydrogen peroxide 50 residual in the multi-walled carbon nano-tubes, the wetting ability multi-walled carbon nano-tubes after finally obtaining handling;
(3) the multi-walled carbon nano-tubes 100mg after step (2) processing is added in the 20ml ethanol, sonic oscillation 2 minutes obtains the higher multi-walled carbon nano-tubes dispersion liquid of stability.
Claims (1)
1. method of utilizing ydrogen peroxide 50 to carry out the surface-functionalized processing of multi-walled carbon nano-tubes is characterized in that concrete steps are:
(1) multi-walled carbon nano-tubes is heated to 100-200 ℃, kept 3-20 hour, to remove partial impurities and moisture content;
(2) the preparation mass percent concentration is the hydrogen peroxide solution 300ml of 1%-30%, adds the multi-walled carbon nano-tubes after 1g step (1) is handled, and handles 5-120 minute with dispersion emulsifying machine; In 60-90 ℃ loft drier, dry, in the evaporation hydrogen peroxide solution, remove ydrogen peroxide 50 residual in the multi-walled carbon nano-tubes, the wetting ability multi-walled carbon nano-tubes after finally obtaining handling;
When (3) using the multi-walled carbon nano-tubes 100mg after step (2) processing is joined in the 20ml ethanol, sonic oscillation 1-5 minute, promptly obtain the carbon nanotube alcohol dispersion liquid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100624720A CN102557011A (en) | 2012-03-09 | 2012-03-09 | Method for performing functionalization treatment to surface of multi-walled carbon nanotube by utilizing hydrogen peroxide |
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| CN2012100624720A CN102557011A (en) | 2012-03-09 | 2012-03-09 | Method for performing functionalization treatment to surface of multi-walled carbon nanotube by utilizing hydrogen peroxide |
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| CN102557011A true CN102557011A (en) | 2012-07-11 |
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| CN2012100624720A Pending CN102557011A (en) | 2012-03-09 | 2012-03-09 | Method for performing functionalization treatment to surface of multi-walled carbon nanotube by utilizing hydrogen peroxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445151A (en) * | 2014-12-02 | 2015-03-25 | 张满锦 | Method for preparing water-soluble multi-walled carbon nanotube |
| EP3147260A4 (en) * | 2014-02-24 | 2017-11-29 | Sekisui Chemical Co., Ltd. | Carbon material, resin composite material, and method for producing said carbon material and resin composite material |
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| CN1513757A (en) * | 2003-07-31 | 2004-07-21 | 上海交通大学 | Preparation method of block polymer grafted earbon nano-pipe |
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
| CN101229918A (en) * | 2008-01-18 | 2008-07-30 | 北京化工大学 | Oxidation modifying method for carbon nano-tube |
| CN101575096A (en) * | 2009-06-02 | 2009-11-11 | 桂林电子科技大学 | Method for preparing carbon nanotube grafted with vinyl macromolecular chain on the surface |
| CN101580243A (en) * | 2009-06-03 | 2009-11-18 | 惠州市沃特新材料有限公司 | Surface treatment method of carbon nanotube and method for preparing composite plastic by using the same |
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2012
- 2012-03-09 CN CN2012100624720A patent/CN102557011A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
| CN1513757A (en) * | 2003-07-31 | 2004-07-21 | 上海交通大学 | Preparation method of block polymer grafted earbon nano-pipe |
| CN101229918A (en) * | 2008-01-18 | 2008-07-30 | 北京化工大学 | Oxidation modifying method for carbon nano-tube |
| CN101575096A (en) * | 2009-06-02 | 2009-11-11 | 桂林电子科技大学 | Method for preparing carbon nanotube grafted with vinyl macromolecular chain on the surface |
| CN101580243A (en) * | 2009-06-03 | 2009-11-18 | 惠州市沃特新材料有限公司 | Surface treatment method of carbon nanotube and method for preparing composite plastic by using the same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3147260A4 (en) * | 2014-02-24 | 2017-11-29 | Sekisui Chemical Co., Ltd. | Carbon material, resin composite material, and method for producing said carbon material and resin composite material |
| CN104445151A (en) * | 2014-12-02 | 2015-03-25 | 张满锦 | Method for preparing water-soluble multi-walled carbon nanotube |
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Application publication date: 20120711 |
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