CN115558329A - Method for dispersing carbon nano-tubes in wave-absorbing coating system and wave-absorbing coating - Google Patents
Method for dispersing carbon nano-tubes in wave-absorbing coating system and wave-absorbing coating Download PDFInfo
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- CN115558329A CN115558329A CN202211368985.4A CN202211368985A CN115558329A CN 115558329 A CN115558329 A CN 115558329A CN 202211368985 A CN202211368985 A CN 202211368985A CN 115558329 A CN115558329 A CN 115558329A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Abstract
The invention provides a method for dispersing carbon nano tubes in a wave-absorbing coating system, which is characterized in that aggregation and winding of the carbon nano tubes are destroyed by stirring, dispersing, crushing, activating and other effects of a high-speed stirring disperser, and then the surfaces of the carbon nano tubes are adsorbed or chemically treated by organic functional groups of a surfactant on the basis of the aggregation and winding, so that the hydroxyl modified carbon nano tubes are subjected to surface treatment, carbon nano tube materials are not aggregated into blocks, and unique advantages of the carbon nano tubes are fully exerted. The carbon nano tube in the system formed by the invention has the characteristics of easy and uniform dispersion and stable system, and the wave-absorbing coating prepared by the mixture prepared by the method has the advantages of small using amount of the electric conductor, good wave-absorbing performance, excellent oil resistance, corrosion resistance, heat resistance, solvent resistance, stable performance and long service life.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a method for dispersing carbon nano tubes in a wave-absorbing coating system and a wave-absorbing coating.
Background
Since the discovery of 1991, carbon nanotubes have attracted attention day and night due to their unique structures and peculiar physical and chemical properties, such as unique metal or semiconductor conductivity, very high mechanical strength, hydrogen storage capacity, adsorption capacity and strong microwave absorption capacity, and potential application prospects, and have attracted great interest to scientists of various countries, and have become one of the international research hotspots in the fields of physics, chemistry, materials science, and the like.
Application research shows that the carbon nanotube can be used in various high-tech fields, for example, the carbon nanotube can be used as a reinforcing agent and a conductive agent to manufacture an automobile protection part with excellent performance, the carbon nanotube can be used as a catalyst carrier to obviously improve the activity and selectivity of a catalyst, and the carbon nanotube has stronger microwave absorption capacity, so that the carbon nanotube can be used as an absorbent to prepare a stealth material, an electromagnetic shielding material, a darkroom wave-absorbing material and the like.
Carbon nanotubes are considered as a novel functional material and a structural material with excellent performance, and all countries in the world put a great deal of research and development force on preparation and application, and are expected to occupy the highest point of the technical field. However, carbon nanotubes are a nano material and are very easily aggregated, and if they are mixed with a polymer like carbon fibers, the carbon nanotubes are easily aggregated into useless agglomerates, and thus cannot exert their excellent properties.
Disclosure of Invention
The invention aims to solve the problems that the existing carbon nano tubes are easy to aggregate and can be easily aggregated into useless blocks, and the superiority of the existing carbon nano tubes can not be exerted, and provides a method for dispersing the carbon nano tubes in a wave-absorbing coating system.
According to a first aspect of the object of the present invention, there is provided a method for dispersing carbon nanotubes in a wave-absorbing coating system, comprising the steps of:
s1, premixing and reacting a carbon nano tube, a coupling agent and an organic solvent under a stirring state to obtain a first mixed solution; wherein, the carbon nano tube in the first mixed solution is dispersed, crushed and activated;
s2, adding a dispersing agent into the first mixed solution, and uniformly stirring and dispersing to obtain a second mixed solution; wherein, the organic functional group carbon nanotube surface of the dispersant is adsorbed or chemically treated;
and S3, adding bisphenol A epoxy resin into the second mixed solution, and uniformly stirring and dispersing to obtain the bisphenol A epoxy resin.
Preferably, in the step S1, the carbon nanotube is a hydroxyl-modified carbon nanotube, the tube diameter is 8 to 20nm, and the tube length is 10 to 30 μm.
Preferably, in step S1, the coupling agent is at least one of a titanate coupling agent or a silane coupling agent.
Preferably, in the step S1, the organic solvent is at least one of xylene, n-butanol, butyl acetate, ethyl acetate or acetone.
Preferably, in the step S1, the rotation speed of stirring is 1000 to 2000rpm, and the stirring time is 20 to 30min.
Preferably, in the step S2, the dispersant is at least one of a polyester modified special compound or a polyacrylate polymer type dispersant.
Preferably, in the step S2, the rotation speed of the stirring is 1000 to 2000rpm, and the stirring time is 40 to 60min.
Preferably, in the step S3, the bisphenol A epoxy resin is at least one of E-44, E-51 or E-55;
the stirring speed is 1000-2000 rpm, and the stirring time is 20-30 min.
According to a second aspect of the invention, the wave-absorbing coating prepared by the method is provided.
Preferably, the wave-absorbing coating is prepared from the following raw materials in parts by weight:
the invention has the beneficial effects that:
the method for dispersing the carbon nano tubes in the wave-absorbing coating system destroys aggregation and winding of the carbon nano tubes by stirring, dispersing, crushing, activating and other effects of the high-speed stirring disperser, and then uses organic functional groups of the surfactant to perform adsorption or chemical treatment on the surfaces of the carbon nano tubes and perform surface treatment on the hydroxyl modified carbon nano tubes, so that the carbon nano tube materials are not aggregated into blocks, and unique advantages of the carbon nano tubes are fully exerted.
The carbon nano tube in the system formed by the invention has the characteristics of easy and uniform dispersion and stable system, and the wave-absorbing coating prepared by the mixture prepared by the method has the advantages of small using amount of the electric conductor, good wave-absorbing performance, excellent oil resistance, corrosion resistance, heat resistance, solvent resistance, stable performance and long service life.
Detailed Description
In order to better understand the technical contents of the present invention, specific embodiments are specifically illustrated as follows.
Embodiments of the present disclosure are not necessarily intended to encompass all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways.
The invention provides a method for dispersing carbon nano tubes in a wave-absorbing coating system, which comprises the following steps:
s1, premixing and reacting a carbon nano tube, a coupling agent and an organic solvent under a stirring state to obtain a first mixed solution; wherein the carbon nanotubes in the first mixed solution are dispersed, pulverized, and activated.
S2, adding a dispersing agent into the first mixed solution, and uniformly stirring and dispersing to obtain a second mixed solution; wherein the organic functional group of the dispersant is used for carrying out adsorption or chemical treatment on the surface of the carbon nano tube.
And S3, adding bisphenol A epoxy resin into the second mixed solution, and uniformly stirring and dispersing to obtain the bisphenol A epoxy resin.
In a preferred embodiment, in the step S1, the carbon nanotubes are hydroxyl-modified carbon nanotubes, the diameter of the tube is 8 to 20nm, and the length of the tube is 10 to 30 μm.
In a preferred embodiment, in the step S1, the coupling agent is at least one of a titanate coupling agent or a silane coupling agent.
In a preferred embodiment, in the step S1, the organic solvent is at least one of xylene, n-butanol, butyl acetate, ethyl acetate or acetone.
In a preferred embodiment, in the step S1, the rotation speed of the stirring is 1000 to 2000rpm, and the stirring time is 20 to 30min.
In a preferred embodiment, in the step S2, the dispersant is at least one of a polyester modified special compound or a polyacrylate polymer type dispersant. For example, CM-3191
In a preferred embodiment, in the step S2, the rotation speed of the stirring is 1000 to 2000rpm, and the stirring time is 40 to 60min.
In a preferred embodiment, in the step S3, the bisphenol A epoxy resin is at least one of E-44, E-51 or E-55;
the stirring speed is 1000-2000 rpm, and the stirring time is 20-30 min.
In another exemplary embodiment of the invention, a wave-absorbing coating prepared by the method is provided.
In a preferred embodiment, the wave-absorbing coating is prepared from the following raw materials in parts by weight:
for better understanding, the present invention is further described below with reference to several specific examples, but the materials and processing techniques are not limited thereto, and the present disclosure is not limited thereto.
Example 1
1.5g of hydroxyl modified carbon nano tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-560 and 15g of mixed solvent of dimethylbenzene and n-butyl alcohol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-51 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nanotube/epoxy resin mixed system formed by the technology has the advantages of easy dispersion of the carbon nanotubes, particularly uniform dispersion and relatively stable system.
Example 2
1.5g of hydroxyl modified carbon nano tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-560 and 15g of mixed solvent of dimethylbenzene and n-butanol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-44 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nanotube/epoxy resin mixed system formed by the technology has the advantages of easy dispersion of the carbon nanotubes, particularly uniform dispersion and relatively stable system.
Example 3
1.5g of hydroxyl modified carbon nano-tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-550 and 15g of mixed solvent of dimethylbenzene and n-butyl alcohol are mixed and reacted for 30min under the stirring state (the rotating speed is 1000 rpm), 1g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed is 1000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-51 is added, the mixture is stirred at high speed (the rotating speed is 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nanotube/epoxy resin mixed system formed by the technology has the advantages of easy dispersion of the carbon nanotubes, particularly uniform dispersion and relatively stable system.
Example 4
1.5g of hydroxyl modified carbon nano-tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-550 and 15g of mixed solvent of dimethylbenzene and n-butyl alcohol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-44 is added, the mixture is stirred at high speed (the rotating speed of 1000 rpm) and dispersed for 20min, and the mixture is mixed uniformly.
The carbon nanotube/epoxy resin mixed system formed by the technology has the advantages of easy dispersion of the carbon nanotubes, particularly uniform dispersion and relatively stable system.
Example 5
1.5g of hydroxyl modified carbon nano tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-560 and 15g of mixed solvent of dimethylbenzene and n-butanol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1g of dispersing agent 3076 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-51 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nano tube/epoxy resin mixed system formed according to the technology has the advantages of easy dispersion of the carbon nano tube, particularly uniform dispersion and relatively stable system.
Example 6
2.0g of hydroxyl modified carbon nano-tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-560 and 15g of mixed solvent of dimethylbenzene and n-butyl alcohol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1.5g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 55g of bisphenol A epoxy resin E-51 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nano tube/epoxy resin mixed system formed according to the technology has the advantages of easy dispersion of the carbon nano tube, particularly uniform dispersion and relatively stable system.
Example 7
2.0g of hydroxyl modified carbon nano-tube with the tube diameter of 8-20 nanometers and the tube length of 10-30 micrometers, 1.5g of silane coupling agent KH-550 and 15g of mixed solvent of dimethylbenzene and n-butyl alcohol are mixed and reacted for 30min under the stirring state (the rotating speed of 2000 rpm), 1.5g of dispersing agent CM-3191 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) by a stirrer and dispersed for 40min, 50g of bisphenol A epoxy resin E-44 is added, the mixture is stirred at high speed (the rotating speed of 2000 rpm) and dispersed for 20min, and the mixture is uniformly mixed.
The carbon nanotube/epoxy resin mixed system formed by the technology has the advantages of easy dispersion of the carbon nanotubes, particularly uniform dispersion and relatively stable system.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (10)
1. A method for dispersing carbon nanotubes in a wave-absorbing coating system is characterized by comprising the following steps:
s1, premixing and reacting a carbon nano tube, a coupling agent and an organic solvent under a stirring state to obtain a first mixed solution; wherein, the carbon nano tube in the first mixed solution is dispersed, crushed and activated;
s2, adding a dispersing agent into the first mixed solution, and uniformly stirring and dispersing to obtain a second mixed solution; wherein, the organic functional group carbon nanotube surface of the dispersant is adsorbed or chemically treated;
and S3, adding bisphenol A epoxy resin into the second mixed solution, and uniformly stirring and dispersing to obtain the bisphenol A epoxy resin.
2. The method for dispersing the carbon nanotubes in the wave-absorbing coating system according to claim 1, wherein in the step S1, the carbon nanotubes are hydroxyl-modified carbon nanotubes, the tube diameter is 8-20 nm, and the tube length is 10-30 μm.
3. The method for dispersing carbon nanotubes in a wave-absorbing coating system according to claim 1, wherein in step S1, the coupling agent is at least one of titanate coupling agent or silane coupling agent.
4. The method for dispersing carbon nanotubes in a wave-absorbing coating system according to claim 1, wherein in step S1, the organic solvent is at least one of xylene, n-butanol, butyl acetate, ethyl acetate or acetone.
5. The method for dispersing the carbon nano tubes in the wave-absorbing coating system according to claim 1, wherein in the step S1, the stirring speed is 1000-2000 rpm, and the stirring time is 20-30 min.
6. The method for dispersing carbon nanotubes in a wave-absorbing coating system according to claim 1, wherein in step S2, the dispersant is at least one of a polyester modified special compound or a polyacrylate high molecular type dispersant.
7. The method for dispersing the carbon nano tubes in the wave-absorbing coating system according to claim 1, wherein in the step S2, the stirring speed is 1000-2000 rpm, and the stirring time is 40-60 min.
8. The method for dispersing carbon nanotubes in a wave-absorbing coating system according to claim 1, wherein in step S3, the bisphenol a epoxy resin is at least one of E-44, E-51 or E-55;
the stirring speed is 1000-2000 rpm, and the stirring time is 20-30 min.
9. A wave-absorbing coating prepared by the method of any one of claims 1 to 9.
10. The wave-absorbing coating according to claim 9, which is prepared from the following raw materials in parts by weight:
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| CN202211368985.4A CN115558329A (en) | 2022-11-03 | 2022-11-03 | Method for dispersing carbon nano-tubes in wave-absorbing coating system and wave-absorbing coating |
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Citations (6)
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|---|---|---|---|---|
| CN1667040A (en) * | 2005-02-22 | 2005-09-14 | 大庆石油管理局 | Method for surface modification of carbon nanotube and its dispersion method in epoxy resin |
| JP2007297255A (en) * | 2006-05-03 | 2007-11-15 | The Inctec Inc | Dispersion containing carbon nanotubes |
| CN103189311A (en) * | 2010-10-29 | 2013-07-03 | 东丽株式会社 | Method for manufacturing liquid dispersion of carbon-nanotube aggregates |
| JP2016111341A (en) * | 2014-12-03 | 2016-06-20 | 国立大学法人 東京大学 | Electromagnetic wave absorber and film forming paste |
| CN106010142A (en) * | 2016-08-08 | 2016-10-12 | 马晓洁 | Dual-cured wear-resistant single-component epoxy resin coating, and preparation method and use method thereof |
| CN106189578A (en) * | 2016-06-30 | 2016-12-07 | 嘉兴市高正高分子材料有限公司 | A kind of high dispersive type oil system carbon nanotube conducting slurry |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1667040A (en) * | 2005-02-22 | 2005-09-14 | 大庆石油管理局 | Method for surface modification of carbon nanotube and its dispersion method in epoxy resin |
| JP2007297255A (en) * | 2006-05-03 | 2007-11-15 | The Inctec Inc | Dispersion containing carbon nanotubes |
| CN103189311A (en) * | 2010-10-29 | 2013-07-03 | 东丽株式会社 | Method for manufacturing liquid dispersion of carbon-nanotube aggregates |
| JP2016111341A (en) * | 2014-12-03 | 2016-06-20 | 国立大学法人 東京大学 | Electromagnetic wave absorber and film forming paste |
| CN106189578A (en) * | 2016-06-30 | 2016-12-07 | 嘉兴市高正高分子材料有限公司 | A kind of high dispersive type oil system carbon nanotube conducting slurry |
| CN106010142A (en) * | 2016-08-08 | 2016-10-12 | 马晓洁 | Dual-cured wear-resistant single-component epoxy resin coating, and preparation method and use method thereof |
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