CN109592670A - The dispersing method of single-walled carbon nanotube - Google Patents
The dispersing method of single-walled carbon nanotube Download PDFInfo
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- CN109592670A CN109592670A CN201811564342.0A CN201811564342A CN109592670A CN 109592670 A CN109592670 A CN 109592670A CN 201811564342 A CN201811564342 A CN 201811564342A CN 109592670 A CN109592670 A CN 109592670A
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- carbon nanotube
- walled carbon
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
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Abstract
The invention discloses a kind of dispersing method of single-walled carbon nanotube, this method first will mix Two-dimensional Inorganic material quantum dot and polyvinylpyrrolidone PVP, obtain composite dispersing agent, and composite dispersing agent is dissolved in polar solvent by stirring, form colloidal sol；Then single-walled carbon nanotube is added in colloidal sol, by high-speed shearing machine, carries out pre-dispersed processing, obtain pre-dispersed liquid；Pre-dispersed liquid is finally subjected to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion liquid.Two-dimensional Inorganic material quantum dot and PVP are mixed with to obtain composite dispersing agent by preparation method of the present invention, and form colloidal sol to handle single-wall carbon tube, this kind of method is more environmentally-friendly, and safety meets the trend of current Green Chemistry.
Description
Technical field
The present invention relates to new material technology fields, and in particular to a kind of dispersing method of single-walled carbon nanotube.
Background technique
Single-wall carbon tube has in many fields since its special structure has excellent electronics, machinery and mechanical property
There is potential application value, be often used as a kind of universal additive, it is only necessary to which considerably less can a little substantially improve material
Performance.But due to the nanostructure of single-wall carbon tube and intermolecular Van der Waals force, with during be usually associated with reunion
A large amount of agglomeration, limit its enhancing, in terms of application.
Currently, the dispersion of single-wall carbon tube is divided into physical dispersion method, chemical dispersion method and physics and chemistry combines dispersion method,
Wherein,
A. physical dispersion method mainly mill, ball milling, ultrasonic wave etc., physical method dispersion is easy to interrupt single-walled carbon nanotube
With destroy single-walled carbon nanotube structure, to cause defect；
B. chemical dispersion method mainly has addition surfactant, strong acid and strong base washing, and chemical method dispersion can not fully open
The Entangled State of single-walled carbon nanotube, while new functional group can be introduced, reduce electric conductivity；
C. physics and chemistry, which combine dispersion method mainly, the washing of ultrasonic wave strong acid and strong base；
The washing of ultrasonic wave strong acid and strong base is used as most important single-wall carbon tube dispersing method, and method is that ultrasonic treatment is mixed
Carbon pipe after closing sour (concentrated sulfuric acid, concentrated nitric acid) oxidation is dispersed to improve its, but this kind of dispersing method complexity, and operating process
It is middle to need the practical mixed acid to highly acid, it is be easy to cause pollution, and can only guarantee that product is stablized in the short time, is not suitable for industry
Change mass production.
Therefore, the single-wall carbon tube with dispersibility how on a large scale, is effectively controllably prepared, there will be biggish market to answer
With value.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of dispersing method of single-walled carbon nanotube,
It solves existing method complexity, be easy to cause pollution, stability is poor, is not easy the problem of being mass produced.
To achieve the above object, a kind of dispersing method of single-walled carbon nanotube designed by the present invention, comprising the following steps:
A. single-walled carbon nanotube, Two-dimensional Inorganic material quantum are weighed by weight 1:0.05~0.2:2~10:100~200
Point, polyvinylpyrrolidone PVP and polar solvent, it is spare；
B. Two-dimensional Inorganic material quantum dot and polyvinylpyrrolidone PVP are mixed, obtains composite dispersing agent, composite diffusion
Agent is dissolved in polar solvent by stirring, forms colloidal sol；
C. single-walled carbon nanotube is added in above-mentioned colloidal sol, by high-speed shearing machine, carries out pre-dispersed processing, obtains pre-
Dispersion liquid；
D. above-mentioned pre-dispersed liquid is subjected to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion liquid.
Further, in the step a), Two-dimensional Inorganic material quantum dot is graphene quantum dot, graphene oxide quantum
Point, at least one of two-dimentional titanium carbide quantum dot and two-dimentional boron nitride, and the partial size of Two-dimensional Inorganic material quantum dot be 1~
20nm。
Still further, polar solvent is water, N-Methyl pyrrolidone NMP and N, N- dimethyl methyl in the step a)
Any one in amide DMF.
Still further, in the step a), single-walled carbon nanotube, Two-dimensional Inorganic material quantum dot, polyvinylpyrrolidine
Ketone PVP and polar solvent weight ratio are 1:0.1~0.2:4~8:100~150.
Still further, in the step a), single-walled carbon nanotube, Two-dimensional Inorganic material quantum dot, polyvinylpyrrolidine
Ketone PVP and polar solvent weight ratio are 1:0.1:5:100.
Still further, the viscosity of colloidal sol is 500~4000cPs in the step a).
Still further, high speed shear speed is 20~100m/s in the step b).
Still further, high-pressure homogeneous pressure is 400~2400bar in the step c).
Beneficial effects of the present invention:
1. preparation method of the present invention by Two-dimensional Inorganic material quantum dot (graphene quantum dot, graphene oxide quantum dot, two
Tie up titanium carbide quantum dot, at least one of two-dimentional boron nitride, partial size is between 1~20nm) and PVP be mixed with to obtain it is compound
Dispersing agent, and colloidal sol is formed to handle single-wall carbon tube, this kind of method is more environmentally-friendly, and safety meets the trend of current Green Chemistry.
2. involved equipment in preparation method of the present invention, such as high pressure homogenizer, high-speed shearing machine are that laboratory is normal
See equipment, and easy to operate, relative inexpensiveness, is suitble to industrialized production.
3. it is strong that method of the invention prepares single-wall carbon tube dispersion stability, it is easy to be mass produced.
Detailed description of the invention
Fig. 1 is the TEM figure of reunion shape single-wall carbon tube selected by the present invention,
Fig. 2 is the TEM figure of the single-wall carbon tube after dispersion prepared by the present invention；
Fig. 3 is the single-walled carbon nanotube Raman map after dispersion；
Fig. 4 is the absorbance map that single-walled carbon nanotube mass fraction is ten a ten thousandths；
Fig. 5 is centrifuged at 8000r/min for single-walled carbon nanotube and is diluted to 100,000 according to original quality score after forty minutes
/ mono- absorbance map；
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, so as to those skilled in the art understand that.
Embodiment 1
The dispersing method of single-walled carbon nanotube, comprising the following steps:
A. by the polyvinylpyrrolidone of graphene quantum dot and 10 parts of quality that the partial size of 0.05 part of quality is 1~20nm
PVP is mixed, and composite dispersing agent is obtained, and will be obtained composite dispersing agent and is dissolved in the DMF of 200 parts of quality by stirring, is formed
Colloidal sol；Wherein, the viscosity of colloidal sol is 500~4000mPs；
B. the single-walled carbon nanotube of 1 part of quality is added in above-mentioned colloidal sol, is 50m/s high-speed shearing machine by speed,
Pre-dispersed processing is carried out, pre-dispersed liquid is obtained；
C. above-mentioned pre-dispersed liquid is carried out under the conditions of pressure is 400bar to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion
Liquid 1.
Embodiment 2
The dispersing method of single-walled carbon nanotube, comprising the following steps:
A. by the polyvinylpyrrolidine of two-dimentional titanium carbide quantum dot and 2 parts of quality that the partial size of 0.1 part of quality is 1~20nm
Ketone PVP is mixed, and composite dispersing agent is obtained, and will be obtained composite dispersing agent and is dissolved in the DMF of 200 parts of quality by stirring, shape
At colloidal sol；Wherein, the viscosity of colloidal sol is 500~4000mPs；
B. the single-walled carbon nanotube of 1 part of quality is added in above-mentioned colloidal sol, is 20m/s high-speed shearing machine by speed,
Pre-dispersed processing is carried out, pre-dispersed liquid is obtained；
C. above-mentioned pre-dispersed liquid is carried out under the conditions of pressure is 1000bar to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion
Liquid 2.
Embodiment 3
The dispersing method of single-walled carbon nanotube, comprising the following steps:
A. by the polyvinylpyrrolidone of graphene quantum dot and 5 parts of quality that the partial size of 0.2 part of quality is 1~20nm
PVP is mixed, and composite dispersing agent is obtained, and will be obtained composite dispersing agent and is dissolved in the NMP of 100 parts of quality by stirring, is formed
Colloidal sol；Wherein, the viscosity of colloidal sol is 500~4000mPs；
B. the single-walled carbon nanotube of 1 part of quality is added in above-mentioned colloidal sol, is 78m/s high-speed shearing machine by speed,
Pre-dispersed processing is carried out, pre-dispersed liquid is obtained；
C. above-mentioned pre-dispersed liquid is carried out under the conditions of pressure is 1200bar to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion
Liquid 3.
Embodiment 4
The dispersing method of single-walled carbon nanotube, comprising the following steps:
A. by the polyvinylpyrrolidone of graphene quantum dot and 10 parts of quality that the partial size of 0.1 part of quality is 1~20nm
PVP is mixed, and composite dispersing agent is obtained, and will be obtained composite dispersing agent and is dissolved in the NMP of 100 parts of quality by stirring, is formed
Colloidal sol；Wherein, the viscosity of colloidal sol is 500~4000mPs；
B. the single-walled carbon nanotube of 2 parts of quality is added in above-mentioned colloidal sol, is 100m/s high-speed shearing machine by speed,
Pre-dispersed processing is carried out, pre-dispersed liquid is obtained；
C. above-mentioned pre-dispersed liquid is carried out under the conditions of pressure is 2400bar to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion
Liquid 4.
Dispersion liquid prepared by embodiment 3 is diluted to 100,000 according to single-walled carbon nanotube quality as shown in Fig. 1~5/
One, 500nm absorbance are 0.578, and same batch of material is centrifuged 40 minutes under the centrifuge of 8000r/min, according to original quality point
Single-walled carbon nanotube quality is diluted to ten a ten thousandths by number, and absorbance 0.541 maintains original absorbance, institute substantially
Have the characteristics that good dispersion and stability are strong with single-walled carbon nanotube dispersion liquid prepared by the present invention.
Other unspecified parts are the prior art.Although above-described embodiment is made that the present invention and retouches in detail
State, but it is only a part of the embodiment of the present invention, rather than whole embodiments, people can also according to the present embodiment without
Other embodiments are obtained under the premise of creativeness, these embodiments belong to the scope of the present invention.
Claims (8)
1. a kind of dispersing method of single-walled carbon nanotube, it is characterised in that: the following steps are included:
A. by weight 1:0.05~0.2:2~10:100~200 weigh single-walled carbon nanotube, Two-dimensional Inorganic material quantum dot,
Polyvinylpyrrolidone PVP and polar solvent, it is spare；
B. Two-dimensional Inorganic material quantum dot and polyvinylpyrrolidone PVP are mixed, obtains composite dispersing agent, composite dispersing agent is logical
It crosses stirring to be dissolved in polar solvent, forms colloidal sol；
C. single-walled carbon nanotube is added in above-mentioned colloidal sol, by high-speed shearing machine, carries out pre-dispersed processing, obtains pre-dispersed
Liquid；
D. above-mentioned pre-dispersed liquid is subjected to high-pressure homogeneous processing and obtains single-wall carbon tube dispersion liquid.
2. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step a), two-dimentional nothing
Machine material quantum dot is graphene quantum dot, graphene oxide quantum dot, in two-dimentional titanium carbide quantum dot and two-dimentional boron nitride
At least one, and the partial size of Two-dimensional Inorganic material quantum dot is 1~20nm.
3. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step a), polarity is molten
Agent is any one in water, N-Methyl pyrrolidone NMP and n,N-Dimethylformamide DMF.
4. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step a), single wall carbon
Nanotube, Two-dimensional Inorganic material quantum dot, polyvinylpyrrolidone PVP and polar solvent weight ratio are 1:0.1~0.2:4~8:
100~150.
5. the dispersing method of single-walled carbon nanotube according to claim 4, it is characterised in that: in the step a), single wall carbon
Nanotube, Two-dimensional Inorganic material quantum dot, polyvinylpyrrolidone PVP and polar solvent weight ratio are 1:0.1:5:100.
6. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step a), colloidal sol
Viscosity is 500~4000cPs.
7. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step b), cut at a high speed
Cutting speed degree is 20~100m/s.
8. the dispersing method of single-walled carbon nanotube according to claim 1, it is characterised in that: in the step c), high pressure is equal
The pressure of matter is 400~2400bar.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110111924A (en) * | 2019-05-24 | 2019-08-09 | 浙江王点科技有限公司 | A kind of graphene quantum dot and single-walled carbon nanotube composite conducting slurry and preparation method |
| CN111020270A (en) * | 2019-12-19 | 2020-04-17 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
| CN112803025A (en) * | 2021-01-22 | 2021-05-14 | 深圳烯湾科技有限公司 | Preparation method of single-walled carbon nanotube conductive slurry, lithium ion battery negative electrode material and preparation method thereof |
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| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
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| CN110111924A (en) * | 2019-05-24 | 2019-08-09 | 浙江王点科技有限公司 | A kind of graphene quantum dot and single-walled carbon nanotube composite conducting slurry and preparation method |
| CN111020270A (en) * | 2019-12-19 | 2020-04-17 | 陕西科技大学 | CNTs reinforced magnesium-based composite material and preparation method thereof |
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Application publication date: 20190409 |