CN100500558C - Shedding method for carbon nano-tube - Google Patents

Abstract

The invention discloses a method for opening a carbon nano tube, comprising the steps that: the carbon nano tube is dispersed in 1 mol/L trifluoroacetic acid, toluene or 1mol/L nitric acid solution, and agitation is carried out under the condition of ultra audible sound or magnetic force so as to achieve even mixture, then ozone is added into, after certain time of reaction, filtration and washing are carried out, then the carbon nano tube is dried in an oven, and finally the carbon nano tube with open ends is gotten. The invention has simple technique and continuous operation can be achieved, thereby being a high efficient and soft method for obtaining the carbon nano tube with open ends.

Description

A kind of hatch method of carbon nanotube

Technical field

The present invention relates to the modification technique field of inorganic nano material, specifically a kind of hatch method of carbon nanotube.

Background technology

Carbon nanotube has unique physicochemical property, and especially the carrier as monodimension nanometer material has very application prospects.Carbon nanotube all causes the great interest of people at catalysis, nano-probe, nano electron device, bioelectrode, drug delivery, various storage system (Li battery and hydrogen energy source) and hollow nano inner reaction tube.For the filling direction of storage system and carbon nanotube, it is essential opening carbon nanotube.Carbon nanotube mainly is at the condition lower opening of aerobic, such as: gaseous cyaniding: utilize CO ₂Stoichiometric number hour or O under the high temperature ₂Stoichiometric number minute at high temperature; Liquid oxidation method: utilize concentrated nitric acid stoichiometric number hour under reflux state; Utilize polyvinyl alcohol at the following stoichiometric number minute of lesser temps (250 ℃); And the oxidisability of potassium permanganate and potassium bichromate is carried out solution method oxidation opening.Though these methods can effectively be opened carbon nanotube, its productive rate is lower, and the sidewall of carbon nanotube is also had very big infringement.

Summary of the invention

The purpose of this invention is to provide a kind ofly under cold condition, can effectively open the method for carbon nanotube, this method also can be finished the modification to carbon nanotube side-wall, increases the water-soluble of carbon nanotube.

The concrete technical scheme that realizes the object of the invention is:

A kind of hatch method of carbon nanotube is characterized in that it comprises following concrete steps:

A, be 0.3g/50ml, get carbon nanotube, join in 1mol/L trifluoroacetic acid or toluene or the 1mol/L nitric acid solvent by carbon nanotube and solvent ratio;

B, stir under the ultrasonic or magnetic force condition, mixture is mixed at 40～60KHz;

C, feed ozone in said mixture, the flow of ozone speed control is built in 20～60ml/min, the carbon nanotube slow oxidation;

After d, the carbon nanotube oxidation, cut off ozone, change logical oxygen, drive away residual ozone, get the opening carbon nanotube suspension;

E, above-mentioned suspension liquid left standstill 0.5 hour, suction filtration, and washing up to filtrate pH=7, at 40～60 ℃ of baking oven inner drying 10～14h, promptly gets the opening carbon nanotube.

Because ozone has very high oxidation potential, the ozone that blasts just is easy to the two keys of C=C of attack carbon nanotube bending, thereby opens the position with defect structure; Trifluoroacetic acids etc. can increase the oxidizing electrode current potential of ozone on the one hand as effective solvent, increase the solvability of ozone and the dispersiveness of carbon nanotube on the other hand.

The invention has the beneficial effects as follows:

1, carbon nano-tube bundle is scatter, and the pipe cap of part carbon nanotube is opened; Most of fragmenting into than short carbon nanotube from sidewall realized both ends open.

2, the sidewall of carbon nanotube is simultaneously by some water miscible group such as hydroxyl, carboxyl modified.Effectively increase the water-soluble of carbon nanotube.

3, the ozone of Dao Chuing can be utilized once more, can reach the continuous utilization of the energy.

Embodiment

Embodiment 1

A, get the 0.30g carbon nanotube, the 1mol/L trifluoroacetic acid solvent that adds 50ml is in three-necked flask.

B, 40KHz ultrasound condition stir down, and it is mixed.

C, employing ozonizer bubbling in above-mentioned mixed solution feed ozone, and ozone flow velocity 20ml/min makes carbon nanotube slow oxidation 12h.

D, close ozonizer, continued logical oxygen 10 minutes, drive away remaining ozone, the opening carbon nanotube suspension.

E, above-mentioned suspension liquid leave standstill 0.5h, the sand core funnel suction filtration, and washing up to the pH=7 of filtrate, at 60 ℃ baking oven inner drying 10h, gets the opening carbon nanotube, and the specific surface area that records the opening carbon nanotube is 196.7100m ²/ g.

Embodiment 2

A, get the 0.60g carbon nanotube, the toluene that adds 100ml is in three-necked flask.

B, under violent magnetic agitation condition, it is mixed.

C, employing ozonizer bubbling in above-mentioned mixed solution feed ozone, and it is 40ml/min that the speed that the adjusting bubble produces makes the ozone flow velocity, carbon nanotube slow oxidation 8h.

D, close ozonizer, continued logical oxygen 10 minutes, drive away remaining ozone, the opening carbon nanotube suspension.

E, above-mentioned suspension liquid leave standstill 0.5h, the sand core funnel suction filtration, and washing up to the pH=7 of filtrate, at 40 ℃ baking oven inner drying 14h, gets the opening carbon nanotube, and the specific surface area that records the opening carbon nanotube is 119.7270m ²/ g.

Embodiment 3

A, get the 0.30g carbon nanotube, the 1mol/L nitric acid that adds 50ml is in three-necked flask.

B, 60KHz ultrasound condition stir down, and it is mixed.

C, employing ozonizer bubbling in above-mentioned mixed solution feed ozone, and ozone flow velocity 60ml/min makes carbon nanotube slow oxidation 10h.

D, close ozonizer, continued logical oxygen 10 minutes, drive away remaining ozone, the opening carbon nanotube suspension.

E, above-mentioned suspension liquid leave standstill 0.5h, the sand core funnel suction filtration, and washing up to the pH=7 of filtrate, at 50 ℃ baking oven inner drying 12h, gets the opening carbon nanotube, and the specific surface area that records the opening carbon nanotube is 165.0306m ²/ g.

Claims (1)

1, a kind of hatch method of carbon nanotube is characterized in that it comprises following concrete steps:

A, be 0.3g/50ml, get carbon nanotube, join in 1mol/L trifluoroacetic acid or toluene or the 1mol/L nitric acid solvent by carbon nanotube and solvent ratio;

B, stir under the ultrasonic or magnetic force condition, mixture is mixed at 40～60KHz;

C, feed ozone in said mixture, the flow of ozone speed control is built in 20～60ml/min, the carbon nanotube slow oxidation;

After d, the carbon nanotube oxidation, cut off ozone, change logical oxygen, drive away residual ozone, get the opening carbon nanotube suspension;

E, above-mentioned suspension liquid left standstill 0.5 hour, suction filtration, and washing up to filtrate pH=7, at 40～60 ℃ of baking oven inner drying 10～14h, promptly gets the opening carbon nanotube.