CN108384451B - Single-walled carbon nanotube conductive spraying liquid, conductive coating and related preparation method - Google Patents
Single-walled carbon nanotube conductive spraying liquid, conductive coating and related preparation method Download PDFInfo
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- CN108384451B CN108384451B CN201810121336.1A CN201810121336A CN108384451B CN 108384451 B CN108384451 B CN 108384451B CN 201810121336 A CN201810121336 A CN 201810121336A CN 108384451 B CN108384451 B CN 108384451B
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- 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
Abstract
The invention provides a single-walled carbon nanotube conductive spraying liquid which comprises the following components in parts by weight: 1 to 3 parts of single-walled carbon nanotube pre-dispersion, 15 to 20 parts of methyl vinyl siloxane, 2 to 6 parts of white carbon black, 4 to 6 parts of carbon black, 200 to 250 parts of siloxane and 0.3 to 1 part of dispersing auxiliary agent. Single-walled carbon nanotube conductive coatings formed thereby and related methods of preparation are also provided. The conductive coating formed by the single-walled carbon nanotube conductive spraying liquid has the advantages of high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple and convenient preparation and low cost, and is suitable for large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of conductive coatings, in particular to the technical field of conductive spraying liquid for forming a conductive coating, and specifically relates to single-walled carbon nanotube conductive spraying liquid, a conductive coating and related preparation methods.
Background
The current conductive silicone rubber spraying has the following defects:
1. the conductivity was poor and the surface resistance was around 5000 ohms (tested using a multimeter).
2. The aging resistance is poor, the conductivity begins to decay obviously after the storage for 3 months, and the conductivity does not have conductivity after the salt spray test.
3. The traditional conductive coating uses toxic and harmful chemicals such as dimethylbenzene, white gasoline and the like as solvents, and has high toxicity.
4. The conventional conductive coating has decarburization and affects the environment, as shown in fig. 1, which is the surface of the conventional conductive carbon black, and the conventional conductive coating needs a large amount of conductive carbon black, and the carbon black falls off after long-term operation.
5. The electrical conductivity of the parts of the equipment using the conventional conductive coating can cause fatal accidents of the equipment once the parts fail in the long-term operation process.
Therefore, it is necessary to provide a conductive spraying liquid, and a conductive coating formed by using the conductive spraying liquid has high conductivity, good aging resistance, safety and environmental protection.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the single-walled carbon nanotube conductive spraying liquid, and a conductive coating formed by adopting the conductive spraying liquid has high conductivity, good aging resistance, safety and environmental protection, and is suitable for large-scale popularization and application.
The invention also aims to provide the single-walled carbon nanotube conductive spraying liquid which is ingenious in design, simple and convenient to prepare, low in cost and suitable for large-scale popularization and application.
The invention also aims to provide a preparation method of the single-walled carbon nanotube conductive spraying liquid, and a conductive coating formed by the single-walled carbon nanotube conductive spraying liquid prepared by the method has high conductivity, good aging resistance, safety and environmental protection, and is suitable for large-scale popularization and application.
The invention also aims to provide a preparation method of the single-walled carbon nanotube conductive spraying liquid, which has the advantages of ingenious design, simple and convenient operation and low cost and is suitable for large-scale popularization and application.
The invention also aims to provide the single-walled carbon nanotube conductive coating which has high conductivity, good aging resistance, safety and environmental protection and is suitable for large-scale popularization and application.
The invention also aims to provide the single-walled carbon nanotube conductive coating which is ingenious in design, simple and convenient to prepare, low in cost and suitable for large-scale popularization and application.
The invention also aims to provide a preparation method of the single-walled carbon nanotube conductive coating, and the single-walled carbon nanotube conductive coating prepared by the method has high conductivity, good aging resistance, safety and environmental protection, and is suitable for large-scale popularization and application.
The invention also aims to provide a preparation method of the single-walled carbon nanotube conductive coating, which has the advantages of ingenious design, simple and convenient operation and low cost and is suitable for large-scale popularization and application.
In order to achieve the above object, in a first aspect of the present invention, there is provided a single-walled carbon nanotube conductive spray coating solution, which is characterized by comprising the following components and amounts:
preferably, the silicone is a low viscosity methyl siloxane.
Preferably, the dispersing aid is modified silicone oil.
In a second aspect of the present invention, a method for preparing the single-walled carbon nanotube conductive spraying solution is provided, which is characterized by comprising the following steps:
(1) mixing the methyl vinyl siloxane, the white carbon black and the carbon black to prepare a mixed mixture;
(2) grinding the single-walled carbon nanotube pre-dispersion body, the dispersing aid and the mixing mixture to prepare a grinding mixture;
(3) and dispersing the grinding mixture and the siloxane to prepare the single-walled carbon nanotube conductive spraying liquid.
Preferably, in the step (1), the mixing is performed in an internal mixer, the mixing speed is 20 rpm, the mixing time is 2 hours, and the mixing temperature is 150 ℃.
Preferably, in the step (2), the grinding is performed on a three-roll grinder, the number of grinding passes is 20, and the roll gap of the three-roll grinder is 1 micron.
Preferably, in the step (3), the dispersion is performed in an ultra high speed disperser, the rotation speed of the dispersion is 2500 rpm, the dispersion time is 2 hours, and the temperature of the dispersion is room temperature.
In a third aspect of the present invention, a single-walled carbon nanotube conductive coating is provided, which is characterized by comprising the single-walled carbon nanotube conductive spraying liquid, and the following components and amounts:
2 to 5 parts by weight of curing agent.
Preferably, the curing agent is a platinum complex.
In a fourth aspect of the present invention, a method for preparing the conductive coating of the single-walled carbon nanotube is provided, which is characterized by comprising the following steps:
(A) and adding the curing agent into the single-walled carbon nanotube conductive spraying liquid, uniformly stirring, spraying the mixture on the surface of a product to be sprayed, and baking to form the single-walled carbon nanotube conductive coating.
Preferably, in the step (a), the baking temperature is 180 ℃, and the baking time is 10 minutes.
Preferably, the article to be sprayed is a silicone rubber article.
The invention has the following beneficial effects:
1. the single-walled carbon nanotube conductive spraying liquid comprises the following components in parts by weight: 1-3 parts of single-walled carbon nanotube pre-dispersion, 15-20 parts of methyl vinyl siloxane, 2-6 parts of white carbon black, 4-6 parts of carbon black, 200-250 parts of siloxane and 0.3-1 part of dispersing auxiliary agent, so that the conductive coating formed by the conductive spraying liquid has high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple and convenient preparation and low cost, and is suitable for large-scale popularization and application.
2. The preparation method of the single-walled carbon nanotube conductive spraying liquid comprises the following steps: (1) mixing methyl vinyl siloxane, white carbon black and carbon black to prepare a mixed mixture; (2) grinding the single-walled carbon nanotube pre-dispersion body, the dispersing auxiliary agent and the mixed mixture to prepare a ground mixture; (3) the grinding mixture and siloxane are dispersed into the single-walled carbon nanotube conductive spraying liquid, so that the conductive coating formed by the single-walled carbon nanotube conductive spraying liquid prepared by the method has high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple and convenient operation and low cost, and is suitable for large-scale popularization and application.
3. The single-walled carbon nanotube conductive coating comprises single-walled carbon nanotube conductive spraying liquid, the following components and the following using amounts: 2 to 5 parts by weight of curing agent, therefore, the conductive epoxy resin composition has high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple preparation and low cost, and is suitable for large-scale popularization and application.
4. The preparation method of the single-walled carbon nanotube conductive coating comprises the following steps: (A) the curing agent is added into the single-walled carbon nanotube conductive spraying liquid, the mixture is uniformly stirred and sprayed on the surface of a product to be sprayed, and the single-walled carbon nanotube conductive coating is formed by baking, so that the single-walled carbon nanotube conductive coating prepared by the method has the advantages of high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple and convenient operation, low cost and suitability for large-scale popularization and application.
These and other objects, features and advantages of the present invention will become more fully apparent from the following detailed description, the accompanying drawings and the claims, and may be realized by means of the instrumentalities, devices and combinations particularly pointed out in the appended claims.
Drawings
Fig. 1 is a schematic surface view of a conventional conductive carbon black.
FIG. 2 is a schematic representation of the fiberized surface structure of one embodiment of the single wall carbon nanotube conductive coating of the present invention.
Figure 3 is a schematic representation of the fiberized surface structure of another embodiment of the single wall carbon nanotube conductive coating of the present invention.
Detailed Description
The present inventors have conducted intensive studies on a conductive coating in order to increase the conductivity of the conductive coating, improve the aging resistance of the conductive coating, and reduce the toxicity of the conductive coating, thereby providing a single-walled carbon nanotube conductive spray solution for forming a single-walled carbon nanotube conductive coating, comprising the following components and amounts:
the silicone may be any suitable silicone, and in one embodiment of the invention, the silicone is a low viscosity methyl siloxane. The low viscosity methylsiloxane has a viscosity of less than 50 centistokes.
The dispersing aid may be any suitable dispersing aid, and in one embodiment of the invention, the dispersing aid is a modified silicone oil.
Also provides a preparation method of the single-walled carbon nanotube conductive spraying liquid, which comprises the following steps:
(1) mixing the methyl vinyl siloxane, the white carbon black and the carbon black to prepare a mixed mixture;
(2) grinding the single-walled carbon nanotube pre-dispersion body, the dispersing aid and the mixing mixture to prepare a grinding mixture;
(3) and dispersing the grinding mixture and the siloxane to prepare the single-walled carbon nanotube conductive spraying liquid.
The mixing can be carried out under any suitable mixing conditions, and in one embodiment of the invention, in the step (1), the mixing is carried out in an internal mixer at a speed of 20 rpm for 2 hours at a temperature of 150 ℃. The mixing temperature is basically about 150 ℃.
The grinding may be carried out using any suitable grinding conditions, and in one embodiment of the invention, in step (2), the grinding is carried out on a three-roll grinder, the number of passes of the grinding being 20, the roll gap of the three-roll grinder being 1 micron. The roll gap of the three-roll mill is substantially around 1 micron.
The dispersion may be carried out using any suitable dispersion conditions, and in one embodiment of the present invention, in the step (3), the dispersion is carried out in an ultra-high speed disperser, the rotation speed of the dispersion is 2500 rpm, the dispersion time is 2 hours, and the dispersion temperature is room temperature.
Also provides a single-walled carbon nanotube conductive coating, which comprises the single-walled carbon nanotube conductive spraying liquid, and the following components and dosage:
2 to 5 parts by weight of curing agent.
The curing agent may be any suitable curing agent, and in one embodiment of the invention, the curing agent is a platinum complex.
Also provides a preparation method of the single-walled carbon nanotube conductive coating, which comprises the following steps:
(A) and adding the curing agent into the single-walled carbon nanotube conductive spraying liquid, uniformly stirring, spraying the mixture on the surface of a product to be sprayed, and baking to form the single-walled carbon nanotube conductive coating.
The baking may be performed under any suitable baking conditions, and in one embodiment of the present invention, in the step (a), the baking temperature is 180 ℃ and the baking time is 10 minutes.
The article to be sprayed may be any suitable article to be sprayed, and in one embodiment of the present invention, the article to be sprayed is a silicone rubber article.
In order to clearly understand the technical contents of the present invention, the following examples are given in detail. Wherein:
single-walled carbon nanotube predispersion (Shanghai Du New Material science and technology Co., Ltd., carbon nanotube dispersion, DMCNTMX-01)
Methyl vinyl siloxane (Dongguan eucalyptus silica gel science and technology Co., Ltd., vinyl silicone oil, TNVF-500)
White carbon black (white carbon black QS-20, chemical industry of De shan Jiang Zhe, Ltd.)
Carbon black (Special high, conductive carbon black, 260G)
Siloxanes (Low viscosity methylsiloxanes) (Dow Corning, methylsilicone oil, PMX-50)
Dispersing auxiliary (modified silicone oil) (Xinyue, modified silicone oil, KP-356)
Curing agent (platinum complex) (Guangzhou silicon friend, platinum vulcanizing agent, PT-500)
Internal mixer (Rugao kun hong kneading machine, vacuum kneader, NHZ-3)
Three-roller grinder (Changzhou city English intelligent machine, three-roller grinder, S65)
Ultra-high speed disperser (Shanghai modern environmental engineering Co., Ltd., ultra-high speed disperser, SFJ-400)
Universal meter (Fuluke, universal meter, 101-600V)
Example 1
1 part of single-walled carbon nanotube pre-dispersion, 20 parts of methyl vinyl siloxane, 4 parts of white carbon black, 6 parts of carbon black, 200 parts of siloxane, 0.5 part of dispersing aid and 5 parts of curing agent.
Adding methyl vinyl siloxane, white carbon black and carbon black into an internal mixer, mixing for 2 hours at the speed of 20 r/min, and controlling the temperature to be about 150 ℃. After the kneading, the mixture was cooled to room temperature to prepare a kneaded mixture.
The single-walled carbon nanotube pre-dispersion, the above-mentioned kneaded mixture and the dispersion aid were ground 20 times (roll gap was about 1 μm) on a three-roll mill to prepare a ground mixture.
Dispersing the grinding mixture and siloxane for 2 hours (the rotating speed is 2500 rpm, the temperature is room temperature) by using an ultra-high speed dispersion machine to prepare the single-walled carbon nanotube conductive spraying liquid.
Before use, the single-walled carbon nanotube conductive spraying liquid is added with a curing agent and stirred uniformly, and then the single-walled carbon nanotube conductive spraying liquid can be sprayed on the surface of a silicon rubber product and baked for 10 minutes at 180 ℃ to form a single-walled carbon nanotube conductive coating, wherein the surface structure of the single-walled carbon nanotube conductive coating is shown in fig. 2.
Example 2
2 parts of single-walled carbon nanotube pre-dispersion, 15 parts of methyl vinyl siloxane, 6 parts of white carbon black, 4 parts of carbon black, 250 parts of siloxane, 0.3 part of dispersing aid and 4 parts of curing agent.
Adding methyl vinyl siloxane, white carbon black and carbon black into an internal mixer, mixing for 2 hours at the speed of 20 r/min, and controlling the temperature to be about 150 ℃. After the kneading, the mixture was cooled to room temperature to prepare a kneaded mixture.
The single-walled carbon nanotube pre-dispersion, the above-mentioned kneaded mixture and the dispersion aid were ground 20 times (roll gap was about 1 μm) on a three-roll mill to prepare a ground mixture.
Dispersing the grinding mixture and siloxane for 2 hours (the rotating speed is 2500 rpm, the temperature is room temperature) by using an ultra-high speed dispersion machine to prepare the single-walled carbon nanotube conductive spraying liquid.
Before use, the single-walled carbon nanotube conductive spraying liquid is added with a curing agent and stirred uniformly, and then the single-walled carbon nanotube conductive spraying liquid can be sprayed on the surface of a silicon rubber product and baked for 10 minutes at 180 ℃ to form a single-walled carbon nanotube conductive coating, wherein the surface structure of the single-walled carbon nanotube conductive coating is shown in fig. 3.
Example 3
3 parts of single-walled carbon nanotube pre-dispersion, 18 parts of methylvinylsiloxane, 2 parts of white carbon black, 5 parts of carbon black, 220 parts of siloxane, 1 part of dispersing aid and 2 parts of curing agent.
Adding methyl vinyl siloxane, white carbon black and carbon black into an internal mixer, mixing for 2 hours at the speed of 20 r/min, and controlling the temperature to be about 150 ℃. After the kneading, the mixture was cooled to room temperature to prepare a kneaded mixture.
The single-walled carbon nanotube pre-dispersion, the above-mentioned kneaded mixture and the dispersion aid were ground 20 times (roll gap was about 1 μm) on a three-roll mill to prepare a ground mixture.
Dispersing the grinding mixture and siloxane for 2 hours (the rotating speed is 2500 rpm, the temperature is room temperature) by using an ultra-high speed dispersion machine to prepare the single-walled carbon nanotube conductive spraying liquid.
The single-walled carbon nanotube conductive spraying liquid is added with a curing agent before use and is uniformly stirred, and then the single-walled carbon nanotube conductive spraying liquid can be sprayed on the surface of a silicon rubber product and is baked for 10 minutes at 180 ℃ to form a single-walled carbon nanotube conductive coating.
Example 4
The surface resistances of the single-walled carbon nanotube conductive coatings of examples 1 to 3 were measured using a multimeter, and the surface resistances of the single-walled carbon nanotube conductive coatings of examples 1 to 3 were 490 ohm, 498 ohm, and 450 ohm, respectively, and thus, the surface resistance was improved to 500 ohm (ranging from 5000 ohm to 10000 ohm to within 500 ohm).
The sprayed products of examples 1 to 3 were subjected to an aging resistance test using an aging resistance test method (the single-walled carbon nanotube conductive coatings of examples 1 to 3 were placed in an oven and baked at 150 ℃ for 72 hours, taken out and cooled to room temperature, and the surface resistance thereof was tested using a multimeter), and the sprayed products of examples 1 to 3 were stored for 1 year without any deterioration in the conductivity of the single-walled carbon nanotube conductive coatings, and were excellent in aging resistance.
Therefore, the single-walled carbon nanotube is used for replacing conductive carbon black as a conductive material for spraying the conductive silicone rubber; the siloxane is used for replacing dimethylbenzene to be used as a solvent for spraying the conductive silicone rubber, and once the traditional conductive spraying uses an environment-friendly solvent, the traditional conductive spraying basically has no conductive performance; solves the problem that the single-walled carbon nanotubes are difficult to disperse in an organic silicon system (which is a worldwide problem and is a barrier that the single-walled carbon nanotubes cannot be used in a large scale in the world). The invention improves the conductivity of the conductive coating, improves the aging resistance and reduces the toxicity.
In conclusion, the conductive coating formed by the single-walled carbon nanotube conductive spraying liquid has high conductivity, good aging resistance, safety, environmental protection, ingenious design, simple and convenient preparation and low cost, and is suitable for large-scale popularization and application.
It will thus be seen that the objects of the invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the embodiments, and the embodiments may be modified without departing from the principles. Therefore, this invention includes all modifications encompassed within the spirit and scope of the claims.
Claims (10)
1. The single-walled carbon nanotube conductive spraying liquid is characterized by comprising the following components in parts by weight:
2. the single-walled carbon nanotube conductive spray coating fluid of claim 1, wherein the dispersion aid is a modified silicone oil.
3. A method for preparing the swnt of any one of claims 1-2, comprising the steps of:
(1) mixing the methyl vinyl polysiloxane, the white carbon black and the carbon black to prepare a mixed mixture;
(2) grinding the single-walled carbon nanotube pre-dispersion body, the dispersing aid and the mixing mixture to prepare a grinding mixture;
(3) and dispersing the grinding mixture and the low-viscosity methyl siloxane to prepare the single-walled carbon nanotube conductive spraying liquid.
4. The method for preparing the single-walled carbon nanotube conductive spray coating liquid of claim 3, wherein in the step (1), the mixing is performed in an internal mixer, the mixing speed is 20 rpm, the mixing time is 2 hours, and the mixing temperature is 150 ℃.
5. The method for preparing the single-walled carbon nanotube conductive spray coating liquid of claim 3, wherein in the step (2), the grinding is performed on a three-roll grinder, the number of grinding passes is 20, and the roll gap of the three-roll grinder is 1 micron.
6. The method for preparing the swnt conductive spraying solution according to claim 3, wherein in the step (3), the dispersion is performed in a super high speed disperser, the rotation speed of the dispersion is 2500 rpm, the dispersion time is 2 hours, and the dispersion temperature is room temperature.
7. A single-walled carbon nanotube conductive coating, comprising the single-walled carbon nanotube conductive spray coating liquid of any one of claims 1-2, and the following components and amounts:
2 to 5 parts by weight of a platinum complex.
8. A method of preparing the conductive coating of single-walled carbon nanotubes of claim 7, comprising the steps of:
(A) and adding the platinum complex into the single-walled carbon nanotube conductive spraying liquid, uniformly stirring, spraying the mixture on the surface of a product to be sprayed, and baking to form the single-walled carbon nanotube conductive coating.
9. The method of claim 8, wherein in step (a), the baking temperature is 180 ℃ and the baking time is 10 minutes.
10. The method of making a single wall carbon nanotube conductive coating of claim 8, wherein the article to be sprayed is a silicone rubber article.
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| CN111312430A (en) * | 2020-02-25 | 2020-06-19 | 深圳市三顺纳米新材料股份有限公司 | Carbon nanotube conductive agent and preparation method thereof |
| CN111718672B (en) * | 2020-06-11 | 2021-11-05 | 南京艾布纳密封技术股份有限公司 | High-performance organic silicon conductive shielding adhesive and preparation method thereof |
| CN113528009A (en) * | 2021-08-04 | 2021-10-22 | 苏州纳普乐思纳米材料有限公司 | Conductive and antistatic liquid and preparation method thereof |
| CN114410143B (en) * | 2022-03-30 | 2022-10-11 | 山东多驰材料科技有限公司 | Static-conducting continuous composite internal anti-corrosion steel pipe and manufacturing method thereof |
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| CN103031058B (en) * | 2012-12-31 | 2015-06-03 | 武汉今福科技有限公司 | Room temperature vulcanized silicone rubber electromagnetic shielding paint and preparation method thereof |
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