CN106189376A - Carbon nanotube dust pretreating process - Google Patents
Carbon nanotube dust pretreating process Download PDFInfo
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- CN106189376A CN106189376A CN201610528845.7A CN201610528845A CN106189376A CN 106189376 A CN106189376 A CN 106189376A CN 201610528845 A CN201610528845 A CN 201610528845A CN 106189376 A CN106189376 A CN 106189376A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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Abstract
The invention discloses a kind of carbon nanotube dust pretreating process: be dissolved in solvent by dispersant, obtain dispersant solution, then dispersant solution is sprayed into by high-pressure spraying method in the CNT of high-speed stirred, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.After the present invention carries out pretreatment to CNT, the bulk density of CNT can be improved, to obtain optimal dispersion effect and good processability.
Description
One, technical field
The present invention relates to a kind of carbon nanotube dust pretreating process
Two, background technology
CNT (Carbon Nanotube, CNT) is one of important member of carbon-based material.Recent two decades comes, carbon system
Material, including carbon fiber, fullerene, CNT, Graphene is found and in succession by as new material application, panoramic
Material with carbon element is just supporting from telecommunications to space flight military project, then to each big field such as biological medicine and new forms of energy, allows them become
Vividly, solid is got up.
CNT has broad application prospects, such as: can apply to rubber, engineering plastics, synthetic resin etc. multiple
Improve the mechanical property of material on condensation material, play potentiation;Can be additionally used in and prepare conductive material, electromagnetic shielding material, lithium electricity
Pond, fuel cell, the electrode modification of colloid lead-acid battery, and novel high speed photoelectric sensor etc.;CNT can also carry
The heat conductivity of high polymer material.
In order to realize above material functional, it is necessary to realize good point in polymeric material matrix of CNT
Dissipate.But, owing to CNT is a kind of high degree of polarization, ganoid inorganic macromolecule compound, few surface defects, shortage
, between CNT, there is stronger Van der Waals force and its huge specific surface area, the highest draw ratio in active group simultaneously,
Causing in the ordinary course of things, CNT is easily wound around reunion bunchy.CNT premium properties to be played makes it extensively apply, as
What solves the dispersion of CNT is critical problem.
Three, summary of the invention
The invention provides a kind of carbon nanotube dust pretreating process, by carbon nano tube surface is carried out pretreatment,
Make carbon nano tube surface activate, obtain the carbon nanotube dust that dispersibility is good with processability.
The technical solution used in the present invention is:
A kind of carbon nanotube dust pretreating process, described technique is:
Dispersant is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed into by high-pressure spraying method
In the CNT of high-speed stirred, after high-speed stirred mixing, prepare Activated Carbon Nanotubes;
Described dispersant is dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, xanthan gum, dodecyl
Sodium sulfate, Triton X-100, sodium carboxymethyl cellulose, Dihexadecylphosphate, arabic gum, cetyl front three
One in base ammonium bromide, alkyl phenol ethylene oxide condensation substance emulsifying agent, cetyl trimethyl sodium bromide, Kynoar or
Two or more mixture;
Described solvent be water, N,N-dimethylformamide, N-Methyl pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, third
One or more mixture in ketone, petroleum ether, ethyl acetate, butyl acetate;
Described CNT, dispersant, the mass fraction ratio of solvent are 85~95:0.1~5:5~10.
Described CNT is one or both the mixture in multi-walled carbon nano-tubes, SWCN.
Described high-pressure spraying method is that with the form of spraying, dispersant solution is sprayed into high-speed stirred by high-pressure spray device
CNT, described high-pressure spray device can use high-pressure spraying machine, by high-pressure hydraulic pump by dispersant solution through high pressure spray
Head becomes spray form to spray in material.Described high-pressure spraying machine still belongs to the first time for CNT pretreating process.High-pressure spraying method
Dispersant solution is atomized, obtains a large amount of fine droplet after atomization, significantly increase the contact area of solution and CNT, have
Beneficially carbon nanotube particulate, by dispersant-coated, strengthens its dispersibility.
In described high-pressure spraying method, spray rate is generally 10~100ml/min;
Atomized particle size is 0.1~1um.
High-speed stirred of the present invention refers to that rotating speed is 300~1500r/min.
The time of described high-speed stirred mixing is generally 1 minute~1 hour, preferably 5~40 minutes.
The auxiliary agent such as surfactant, dispersant is dissolved in suitable solvent by the present invention, by high-pressure spraying method by it
Spray in the CNT of high-speed stirred, cause to be formed between CNT and repel, improve the dispersibility of CNT, and energy
Improve the bulk density of CNT simultaneously, solve existing CNT and easily reunite difficult dispersion and course of processing CNT
The present situation easily dispersed.
After the Activated Carbon Nanotubes that the present invention prepares adds dispersant solution under high velocity agitation, there is certain stickiness, can lead to
Cross single screw extrusion machine and extrude pelletizing, beneficially following process production at normal temperatures.
The present invention carries out high-speed stirred to CNT, to its surface pretreatment, simultaneously by dispersant, surface activity
The auxiliary agents such as agent are dissolved in liquid in the carbon nanotube dust being sprayed in stirring by the way of spraying so that CNT table
Face activates, and simultaneously by the material uniform wet such as dispersant, surfactant, causes to be formed between CNT and repels, improve
The dispersibility of CNT, and the bulk density of CNT can be improved, to obtain optimal dispersion effect with good simultaneously
Processability.
Four, detailed description of the invention
With specific embodiment, technical scheme is described further below, but the protection content of the present invention is not
It is limited to this.
Embodiment 1~16
According to the form below 1 takes each raw material, is dissolved in solvent by dispersant, obtains dispersant solution, is then led to by dispersant solution
Cross high pressure spray process and spray into the CNT (diameter 1~30nm, length 1~100 μm, bulk density 0.02g/mL) of high-speed stirred
In, technological parameter is as shown in table 1, after high-speed stirred mixing, prepares Activated Carbon Nanotubes;
Table 1
The performance test results such as table 2 below of the Activated Carbon Nanotubes prepared
Table 2
Dispersibility experiment detection by the following method: the Activated Carbon Nanotubes 10mg that embodiment 1~16 prepares is separately added into
10mL prepares in the solvent (seeing table 1) used by this Activated Carbon Nanotubes, and ultrasonic disperse 30 minutes obtains suspension, stands, goes out
When being the most substantially layered, the record time is the holding time, and acquired results refers to table 2.Holding time is the longest, shows that its dispersibility is more
Good.The most pretreated CNT cannot form stable suspension.
Above-mentioned test result indicate that, after pretreatment, the bulk density of CNT improve about 10 times (untreated
The bulk density of CNT is about 0.02g/mL), dispersibility is all significantly increased.
Claims (8)
1. a carbon nanotube dust pretreating process, it is characterised in that described technique is:
Dispersant is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed at a high speed by high-pressure spraying method
In the CNT of stirring, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.
2. technique as claimed in claim 1, it is characterised in that described dispersant is dodecylbenzene sodium sulfonate, polyvinyl pyrrole
Alkanone, polyvinyl alcohol, xanthan gum, sodium lauryl sulphate, Triton X-100, sodium carboxymethyl cellulose, double 16
Alkyl phosphoric acid, arabic gum, cetyl trimethylammonium bromide, alkyl phenol ethylene oxide condensation substance emulsifying agent, cetyl three
One or more mixture in methyl bromide sodium, Kynoar.
3. technique as claimed in claim 1, it is characterised in that described solvent is water, DMF, N-methyl pyrrole
In pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, acetone, petroleum ether, ethyl acetate, butyl acetate one or more
Mixture.
4. technique as claimed in claim 1, it is characterised in that described CNT, dispersant, the mass fraction ratio of solvent are
85~95:0.1~5:5~10.
5. technique as claimed in claim 1, it is characterised in that described CNT is multi-walled carbon nano-tubes, SWCN
In one or both mixture.
6. technique as claimed in claim 1, it is characterised in that described high-pressure spraying method is that dispersant solution is passed through high pressure spray
Shower device sprays into the CNT of high-speed stirred with the form of spraying.
7. technique as claimed in claim 1, it is characterised in that in described high-pressure spraying method, spray rate is 10~100ml/
min;Atomized particle size is 0.1~1um.
8. technique as claimed in claim 1, it is characterised in that the rotating speed of described high-speed stirred is 300-1500r/min.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107628688A (en) * | 2017-09-25 | 2018-01-26 | 浙江工业大学 | Multi-walled carbon nanotube is used for the purposes for reducing Water phosphorus |
CN111094180A (en) * | 2018-01-29 | 2020-05-01 | Lg化学株式会社 | Method for producing carbon nanotube dispersions |
CN115448296A (en) * | 2022-09-05 | 2022-12-09 | 烟台大学 | Large-scale rapid gas-phase dispersion method for carbon nanotubes |
Citations (4)
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CN101549866A (en) * | 2009-05-14 | 2009-10-07 | 上海交通大学 | Method for decomposing carbon nano-tube bundle based on high voltage electrostatic spray method |
CN102850628A (en) * | 2012-09-18 | 2013-01-02 | 浙江新大塑料管件有限公司 | Carbon-nano-tube-reinforced polyethylene tube |
CN104479410A (en) * | 2014-11-03 | 2015-04-01 | 重庆和泰塑胶股份有限公司 | Calcium carbonate surface treatment method |
CN104559187A (en) * | 2015-02-03 | 2015-04-29 | 国家电网公司 | Preparation method of carbon nanotube modified organic silicon resin based composite material |
-
2016
- 2016-06-30 CN CN201610528845.7A patent/CN106189376A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101549866A (en) * | 2009-05-14 | 2009-10-07 | 上海交通大学 | Method for decomposing carbon nano-tube bundle based on high voltage electrostatic spray method |
CN102850628A (en) * | 2012-09-18 | 2013-01-02 | 浙江新大塑料管件有限公司 | Carbon-nano-tube-reinforced polyethylene tube |
CN104479410A (en) * | 2014-11-03 | 2015-04-01 | 重庆和泰塑胶股份有限公司 | Calcium carbonate surface treatment method |
CN104559187A (en) * | 2015-02-03 | 2015-04-29 | 国家电网公司 | Preparation method of carbon nanotube modified organic silicon resin based composite material |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107628688A (en) * | 2017-09-25 | 2018-01-26 | 浙江工业大学 | Multi-walled carbon nanotube is used for the purposes for reducing Water phosphorus |
CN111094180A (en) * | 2018-01-29 | 2020-05-01 | Lg化学株式会社 | Method for producing carbon nanotube dispersions |
US11453592B2 (en) | 2018-01-29 | 2022-09-27 | Lg Chem, Ltd. | Method for preparing carbon nanotube dispersion |
CN111094180B (en) * | 2018-01-29 | 2023-03-31 | Lg化学株式会社 | Method for producing carbon nanotube dispersions |
CN115448296A (en) * | 2022-09-05 | 2022-12-09 | 烟台大学 | Large-scale rapid gas-phase dispersion method for carbon nanotubes |
CN115448296B (en) * | 2022-09-05 | 2024-04-12 | 烟台大学 | Large-scale rapid gas-phase dispersion method for carbon nanotubes |
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Application publication date: 20161207 |