CN108423653A - A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function - Google Patents
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function Download PDFInfo
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- CN108423653A CN108423653A CN201810472443.9A CN201810472443A CN108423653A CN 108423653 A CN108423653 A CN 108423653A CN 201810472443 A CN201810472443 A CN 201810472443A CN 108423653 A CN108423653 A CN 108423653A
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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Abstract
The present invention is a kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：Catalyst is added in tube furnace, carrier gas is passed through into tube furnace；Tube furnace is warming up to 800 900 DEG C；Acetylene gas is passed through into tube furnace, the time being passed through is 50min, is then shut off acetylene；After reaction, product carbon nanotube is taken out；By the carbon nanotube of synthesis respectively with ultrasonic cleaning after toluene, acetone soak, filtered product is dried spare for 24 hours in vacuum drying chamber；Carbon nanotube is fitted into three-necked flask, aniline-water solution, hydrochloric acid solution and acetone is added, the ammonium persulfate solution with aniline equivalent is added dropwise with dropping funel under nitrogen protection and ice water cooling, reacts 2h；Filtering is cleaned with dilute hydrochloric acid solution, product dries 12h；Obtain polyaniline in-stiu coating carbon nanotube.After polyaniline in-stiu coating carbon nanotube of the present invention, be conducive to improve its dispersibility, electromagnetic absorption parameter is improved.
Description
Technical field
The field more particularly to a kind of carbon with electromagnetic wave shielding function being synthetically prepared the present invention relates to carbon nanotube are received
The preparation method of mitron.
Background technology
The preparation method of carbon nanotube mainly has arc discharge method, catalystic pyrolysis, laser method, ion beam irradiation at present
Method, solar energy method, electrolysis etc..The application study of carbon nanotube is mainly in energy storage, nano-probe, composite material reinforcement body, work(
It can coating and catalyst carrier etc..When wherein using carbon nanotube as composite material reinforcement body and filler, carbon nanotube is tight
Reaggregation, the problem of being difficult to disperse, cannot preferably solve always, thus limit the performance of its performance.In order to improve its point
Property is dissipated, the oxidation processes such as corona treatment and the concentrated sulfuric acid, concentrated nitric acid are carried out to it, to mount activity in carbon nano tube surface
Functional group, to improve the surface energy state of carbon nanotube and with the chemical reactivity of other substances, but these surface modification sides
Law article part is harsh, it is difficult to prepared by batch.
Invention content
The present invention is directed to improve the surface nature of carbon nanotube, and provide a kind of carbon nanometer with electromagnetic wave shielding function
The preparation method of pipe.
The present invention to achieve the above object, using following technical scheme：
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 800-900 DEG C, heating rate is 20-25 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off second
Alkynes；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used to ultrasonic cleaning after toluene, acetone soak successively, filtered product is in vacuum
Drying is spare for 24 hours in drying box；
S6, the carbon nanotube after drying is fitted into three-necked flask, be added aniline-water solution, 1mol/L hydrochloric acid solution and
The mass ratio of acetone, carbon nanotube and aniline-water solution is 4：1；Nitrogen protection and ice water cooling under with dropping funel be added dropwise with
The ammonium persulfate solution of the 1mol/L of aniline equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate chlorination
Until the titration of barium solution is generated without precipitation, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanometer
Pipe.
Drying temperature in vacuum drying chamber is 60 DEG C.
The catalyst is nickel protoxide powder or ferrocene.
Catalyst is added in tube furnace, and with the lasting process for being passed through carrier gas into tube furnace of the speed of 1L/min
In, nickel sulfide is added as co-catalyst.
The carrier gas is nitrogen or hydrogen.
The beneficial effects of the invention are as follows：After polyaniline in-stiu coating carbon nanotube of the present invention, surface is because carrying polar Asia
Amido makes its surface energy improve, and is conducive to improve its dispersibility.After polyaniline in-stiu coating carbon nanotube, electromagnetic absorption ginseng
Number is improved.
Specific implementation mode
The present invention is further explained in the light of specific embodiments：
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 800-900 DEG C, heating rate is 20-25 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off second
Alkynes；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used to ultrasonic cleaning after toluene, acetone soak successively, filtered product is in vacuum
Drying is spare for 24 hours in drying box；
S6, the carbon nanotube after drying is fitted into three-necked flask, be added aniline-water solution, 1mol/L hydrochloric acid solution and
The mass ratio of acetone, carbon nanotube and aniline-water solution is 4：1；Nitrogen protection and ice water cooling under with dropping funel be added dropwise with
The ammonium persulfate solution of the 1mol/L of aniline equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate chlorination
Until the titration of barium solution is generated without precipitation, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanometer
Pipe.
Drying temperature in vacuum drying chamber is 60 DEG C.
The catalyst is nickel protoxide powder or ferrocene.
Catalyst is added in tube furnace, and with the lasting process for being passed through carrier gas into tube furnace of the speed of 1L/min
In, nickel sulfide is added as co-catalyst.
The carrier gas is nitrogen or hydrogen.
Specific embodiment 1：
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 800 DEG C, heating rate is 20 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off second
Alkynes；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used to ultrasonic cleaning after toluene, acetone soak successively, filtered product is in vacuum
Drying is spare for 24 hours in drying box；
S6, the carbon nanotube after drying is fitted into three-necked flask, be added aniline-water solution, 1mol/L hydrochloric acid solution and
The mass ratio of acetone, carbon nanotube and aniline-water solution is 4：1；Nitrogen protection and ice water cooling under with dropping funel be added dropwise with
The ammonium persulfate solution of the 1mol/L of aniline equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate chlorination
Until the titration of barium solution is generated without precipitation, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanometer
Pipe.
Drying temperature in vacuum drying chamber is 60 DEG C.
The catalyst is nickel protoxide powder.
Catalyst is added in tube furnace, and with the lasting process for being passed through carrier gas into tube furnace of the speed of 1L/min
In, nickel sulfide is added as co-catalyst.
The carrier gas is nitrogen.
Specific embodiment 2：
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 900 DEG C, heating rate is 25 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off second
Alkynes；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used to ultrasonic cleaning after toluene, acetone soak successively, filtered product is in vacuum
Drying is spare for 24 hours in drying box；
S6, the carbon nanotube after drying is fitted into three-necked flask, be added aniline-water solution, 1mol/L hydrochloric acid solution and
The mass ratio of acetone, carbon nanotube and aniline-water solution is 4：1；Nitrogen protection and ice water cooling under with dropping funel be added dropwise with
The ammonium persulfate solution of the 1mol/L of aniline equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate chlorination
Until the titration of barium solution is generated without precipitation, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanometer
Pipe.
Drying temperature in vacuum drying chamber is 60 DEG C.
The catalyst is ferrocene.
Catalyst is added in tube furnace, and with the lasting process for being passed through carrier gas into tube furnace of the speed of 1L/min
In, nickel sulfide is added as co-catalyst.
The carrier gas is hydrogen.
Specific embodiment 3：
A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 850 DEG C, heating rate is 22 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off second
Alkynes；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used to ultrasonic cleaning after toluene, acetone soak successively, filtered product is in vacuum
Drying is spare for 24 hours in drying box；
S6, the carbon nanotube after drying is fitted into three-necked flask, be added aniline-water solution, 1mol/L hydrochloric acid solution and
The mass ratio of acetone, carbon nanotube and aniline-water solution is 4：1；Nitrogen protection and ice water cooling under with dropping funel be added dropwise with
The ammonium persulfate solution of the 1mol/L of aniline equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate chlorination
Until the titration of barium solution is generated without precipitation, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanometer
Pipe.
Drying temperature in vacuum drying chamber is 60 DEG C.
The catalyst is nickel protoxide powder.
Catalyst is added in tube furnace, and with the lasting process for being passed through carrier gas into tube furnace of the speed of 1L/min
In, nickel sulfide is added as co-catalyst.
The carrier gas is nitrogen.
Polyaniline is the conducting polymer composite that adulterates being concerned, and is applied to conducting polymer film in recent years, is made
Conducting resinl and antistatic, corrosion resistant coating and stealth material are prepared for filler.Polyaniline synthesis condition is simple, contains in strand
There is imine group to make it have higher surface energy.After polyaniline in-stiu coating carbon nanotube of the present invention, surface is because of band polarized
Imido grpup, so that its surface energy is improved, be conducive to improve its dispersibility.After polyaniline in-stiu coating carbon nanotube, electromagnetism is inhaled
Parameter is received to be improved.
The present invention is exemplarily described above in conjunction with specific embodiment, it is clear that the present invention implements not by upper
The limitation of mode is stated, if the various improvement of inventive concept and technical scheme of the present invention progress are used, or it is not improved straight
It scoops out for other occasions, within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the carbon nanotube with electromagnetic wave shielding function, which is characterized in that the specific steps are：
S1, catalyst is added in tube furnace, and carrier gas is passed through into tube furnace so that the speed of 1L/min is lasting；
S2, tube furnace is warming up to 800-900 DEG C, heating rate is 20-25 DEG C/min；
S3, acetylene gas is passed through with the speed of 5L/min into tube furnace, the time being passed through is 50min, is then shut off acetylene；
S4, after reaction takes out product carbon nanotube；
S5, the carbon nanotube of synthesis is used successively ultrasonic cleaning after toluene, acetone soak, filtered product are being dried in vacuo
Drying is spare for 24 hours in case；
S6, the carbon nanotube after drying is fitted into three-necked flask, the hydrochloric acid solution and third of aniline-water solution, 1mol/L is added
The mass ratio of ketone, carbon nanotube and aniline-water solution is 4：1；With dropping funel dropwise addition and benzene under nitrogen protection and ice water cooling
The ammonium persulfate solution of the 1mol/L of amine equivalent reacts 2h, the carbon nanotube tentatively coated；
S7, the carbon nanotube tentatively coated obtained in S6 and filtering are cleaned with dilute hydrochloric acid solution, until filtrate is molten with barium chloride
Until the fixed generation without precipitation of drop, product dry 12h in vacuum drying chamber；Obtain polyaniline in-stiu coating carbon nanotube.
2. a kind of preparation method of carbon nanotube with electromagnetic wave shielding function according to claim 1, feature exist
In the drying temperature in vacuum drying chamber is 60 DEG C.
3. a kind of preparation method of carbon nanotube with electromagnetic wave shielding function according to claim 2, feature exist
In the catalyst is nickel protoxide powder or ferrocene.
4. a kind of preparation method of carbon nanotube with electromagnetic wave shielding function according to claim 3, feature exist
In catalyst being added in tube furnace, and during being passed through carrier gas into tube furnace so that the speed of 1L/min is lasting, is added
Nickel sulfide is as co-catalyst.
5. a kind of preparation method of carbon nanotube with electromagnetic wave shielding function according to claim 4, feature exist
In the carrier gas is nitrogen or hydrogen.
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| CN201810472443.9A CN108423653A (en) | 2018-05-17 | 2018-05-17 | A kind of preparation method of the carbon nanotube with electromagnetic wave shielding function |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110491892A (en) * | 2019-08-19 | 2019-11-22 | 德淮半导体有限公司 | Imaging sensor and preparation method thereof |
| EP3859835A4 (en) * | 2018-11-13 | 2021-11-10 | Lg Energy Solution, Ltd. | Anode active material and manufacturing method therefor |
| CN116162238A (en) * | 2023-03-14 | 2023-05-26 | 广州明晖新材料有限公司 | In-situ polymerization preparation method of spinning-grade conductive carbon nanotube nylon composite material |
-
2018
- 2018-05-17 CN CN201810472443.9A patent/CN108423653A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3859835A4 (en) * | 2018-11-13 | 2021-11-10 | Lg Energy Solution, Ltd. | Anode active material and manufacturing method therefor |
| CN110491892A (en) * | 2019-08-19 | 2019-11-22 | 德淮半导体有限公司 | Imaging sensor and preparation method thereof |
| CN116162238A (en) * | 2023-03-14 | 2023-05-26 | 广州明晖新材料有限公司 | In-situ polymerization preparation method of spinning-grade conductive carbon nanotube nylon composite material |
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Application publication date: 20180821 |