CN110951257A - Preparation method of carbon nanotube/silicone rubber composite material with high dielectric property - Google Patents
Preparation method of carbon nanotube/silicone rubber composite material with high dielectric property Download PDFInfo
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- CN110951257A CN110951257A CN201911280437.4A CN201911280437A CN110951257A CN 110951257 A CN110951257 A CN 110951257A CN 201911280437 A CN201911280437 A CN 201911280437A CN 110951257 A CN110951257 A CN 110951257A
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- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
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Abstract
The invention discloses a preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property, which comprises the following steps: (1) adding silicon rubber and natural rubber into a double-roller mixing roll for mixing; (2) obtaining modified carbon nano-tubes; (3) sequentially adding the modified carbon nano tube, the carbon black, the sulfur and the anti-aging agent into the double-roll mixing mill in the step (1), and mixing to obtain a mixed rubber material; (4) injecting the mixed rubber material into a mold, and carrying out hot pressing to obtain a primary rubber; (5) vulcanizing in a flat vulcanizing machine, and naturally cooling to room temperature to obtain the product; according to the invention, the natural rubber and the silicon rubber in a certain mass ratio are compounded for use, so that the advantages of the natural rubber and the silicon rubber can be complemented in mechanical properties, and meanwhile, the dielectric constant of the composite material can be greatly improved under the action of the synergistic modification of the carbon nano tubes, so that the breakdown strength of the prepared composite material is greatly improved.
Description
Technical Field
The invention belongs to the technical field of rubber composite processing, and particularly relates to a preparation method of a carbon nano tube/silicone rubber composite material with high dielectric property.
Background
It is known that Silicone Rubber (SR) is an important member of high-performance synthetic rubber, and has an irreplaceable status in high-tech fields such as modern high-tech technology, aerospace and the like. The silicone rubber is a polymer with Si-O bond units as a main chain and organic groups as side chains. The polymer is obviously different from a polymer taking a C-C bond unit as a main chain in structure and performance, is a typical semi-inorganic semi-organic polymer, and has heat resistance of an inorganic polymer and flexibility of an organic polymer. Compared with other high polymer rubbers, the silicon rubber has the most remarkable characteristic of excellent thermal stability, is widely used as an elastic material in a high-temperature environment, and is widely applied to the fields of aerospace, light industry, chemical industry, textile, machinery, agriculture, transportation, medical treatment and health care and the like.
However, the dielectric properties of silicone rubber are general, which causes the application of silicone rubber in this field to be greatly limited, and therefore, if the dielectric properties of silicone rubber materials are improved, it is a technical problem to be solved.
Disclosure of Invention
The invention is realized by the following technical scheme.
A preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property comprises the following steps:
(1) uniformly mixing 60-65 parts by weight of silicone rubber and 10-15 parts by weight of natural rubber, and then adding the mixture into a double-roll mixing roll for mixing for 6-8 min;
(2) uniformly dispersing 10-15 parts by weight of carbon nanotubes into 58-60 parts by weight of ethanol solution, magnetically stirring for 30-35min, adding diphenylsilanediol accounting for 5-6% of the mass of the carbon nanotubes and a coupling agent accounting for 1.2-1.6%, continuously magnetically stirring for 1-1.2 hours under the condition of water bath heat preservation, carrying out suction filtration, and drying to constant weight to obtain modified carbon nanotubes.
(3) Adding 6-8 parts by weight of modified carbon nano tube, 3-5 parts by weight of carbon black, 1-1.4 parts by weight of sulfur and 1.2-1.6 parts by weight of anti-aging agent into the double-roll mixing mill in the step (1) in sequence, mixing for 8-12min to obtain a mixed rubber material, and gradually sticking, hardening, embrittlement or cracking the silicone rubber composite material under the action of heat, oxygen, ozone, valence-variable metal ions, mechanical stress, light and high-energy rays and the corrosion of other chemical substances, mould and the like;
(4) injecting the mixed rubber material obtained in the step (3) into a mold, and carrying out hot pressing for 10-12min under the conditions that the temperature is 150-;
(5) and (4) putting the primary rubber obtained in the step (4) into a flat vulcanizing machine for vulcanization treatment for 40-50min, and naturally cooling to room temperature to obtain the rubber.
The natural rubber in the step (1) is a first-grade thin white crepe sheet, is white, dry and firm in color, allows slight color depth difference, and does not allow any sign of discoloration, acid odor, dust, crumbs, grit or other foreign substances, oil stains or other stains, oxidation or overheating caused by any reason.
The silicon rubber in the step (1) is BGP1 silicon rubber.
The mass fraction of the ethanol solution in the step (2) is 60%.
And (3) the rotating speed of the magnetic stirring in the step (2) is 1200 r/min.
And (3) the coupling agent in the step (2) is an organosilane coupling agent.
And (3) keeping the temperature of the water bath at 80 ℃ in the step (2).
And (4) the anti-aging agent in the step (3) is an anti-aging agent MB.
The vulcanization treatment conditions in the step (5) are as follows: the temperature was 180 ℃.
According to the technical scheme, the beneficial effects of the invention are as follows:
the preparation method of the carbon nanotube/silicone rubber composite material with high dielectric property provided by the invention has dielectric property, and the mechanical property of pure silicone rubber is weakened by introducing the carbon nanotube, especially the tearing strength is obviously reduced; the invention uses natural rubber and silicon rubber in a certain mass ratio to carry out combination, not only can complement advantages on mechanical property, but also can greatly improve the defect of reduced tearing strength of the silicon rubber caused by the introduction of the carbon nano tube, and can synergistically modify the action of the carbon nano tube, and can greatly improve the dielectric constant of the composite material, thereby greatly improving the breakdown strength of the prepared composite material, and the silicon rubber composite material can be gradually sticky, hardened, crisp or cracked due to the actions of heat, oxygen, ozone, valence-variable metal ions, mechanical stress, light, high-energy rays, and the erosion of other chemical substances, moulds and the like, and the invention can delay the aging substances of rubber polymer compounds and inhibit the oxidation process by adding a certain amount of synergistic action of the antioxidant MB and the modified carbon nano tube, thereby prolonging the service life of the carbon nano tube/silicon rubber composite material product.
Detailed Description
The invention provides a preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property, and a person skilled in the art can use the content for reference and appropriately improve the process parameters to realize the preparation. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
Example 1
A preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property comprises the following steps:
(1) uniformly mixing 60 parts by weight of silicon rubber and 10 parts by weight of natural rubber, and then adding the mixture into a double-roller mixing roll to mix for 6min, wherein the natural rubber is a first-grade thin white crepe sheet, and the silicon rubber is BGP1 silicon rubber;
(2) uniformly dispersing 10 parts by weight of carbon nanotubes into 58 parts by weight of ethanol solution, wherein the mass fraction of the ethanol solution is 60%, magnetically stirring for 30min at the rotating speed of 1200r/min, then adding diphenylsilanediol accounting for 5% of the mass of the carbon nanotubes and an organosilane coupling agent accounting for 1.2%, keeping the temperature in a water bath at 80 ℃, continuing magnetically stirring for 1 hour, then carrying out suction filtration, and drying to constant weight to obtain modified carbon nanotubes;
(3) sequentially adding 6 parts by weight of modified carbon nano tube, 3 parts by weight of carbon black, 1 part by weight of sulfur and 1.2 parts by weight of antioxidant MB into the double-roll mixing mill in the step (1), and mixing for 8min to obtain a mixed rubber material;
(4) injecting the mixed rubber material obtained in the step (3) into a mold, and carrying out hot pressing for 10min under the conditions of the temperature of 150 ℃ and the pressure of 8MPa to obtain a primary rubber;
(5) and (4) putting the primary rubber obtained in the step (4) into a flat vulcanizing machine for vulcanization treatment for 40min at the temperature of 180 ℃, and naturally cooling to room temperature to obtain the rubber.
Example 2
A preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property comprises the following steps:
(1) uniformly mixing 65 parts by weight of silicon rubber and 15 parts by weight of natural rubber, and then adding the mixture into a double-roller mixing roll to mix for 8min, wherein the natural rubber is a first-grade thin white crepe sheet, and the silicon rubber is BGP1 silicon rubber;
(2) uniformly dispersing 15 parts by weight of carbon nanotubes into 60 parts by weight of ethanol solution, wherein the mass fraction of the ethanol solution is 60%, magnetically stirring for 35min at the rotating speed of 1200r/min, then adding diphenyl silanediol accounting for 6% of the mass of the carbon nanotubes and an organosilane coupling agent accounting for 1.6% of the mass of the carbon nanotubes, keeping the temperature of a water bath at 80 ℃, continuing magnetically stirring for 1.2 hours, then carrying out suction filtration, and drying to constant weight to obtain modified carbon nanotubes;
(3) sequentially adding 8 parts by weight of modified carbon nano tube, 5 parts by weight of carbon black, 1.4 parts by weight of sulfur and 1.6 parts by weight of antioxidant MB into the double-roll mixing mill in the step (1), and mixing for 12min to obtain a mixed rubber material;
(4) injecting the mixed rubber material obtained in the step (3) into a mold, and carrying out hot pressing for 12min under the conditions of the temperature of 158 ℃ and the pressure of 9MPa to obtain a primary rubber;
(5) and (4) putting the primary rubber obtained in the step (4) into a flat vulcanizing machine for vulcanization treatment for 50min at the temperature of 180 ℃, and naturally cooling to room temperature to obtain the rubber.
Example 3
A preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property comprises the following steps:
(1) uniformly mixing 62 parts by weight of silicon rubber and 13 parts by weight of natural rubber, and then adding the mixture into a double-roller mixing roll to mix for 7min, wherein the natural rubber is a first-grade thin white crepe sheet, and the silicon rubber is BGP1 silicon rubber;
(2) uniformly dispersing 14 parts by weight of carbon nanotubes into 59 parts by weight of ethanol solution, wherein the mass fraction of the ethanol solution is 60%, magnetically stirring for 32min at the rotating speed of 1200r/min, then adding diphenylsilanediol accounting for 5.5% of the mass of the carbon nanotubes and an organosilane coupling agent accounting for 1.3%, keeping the temperature in a water bath at 80 ℃, continuing magnetically stirring for 1.1 h, then carrying out suction filtration, and drying to constant weight to obtain modified carbon nanotubes;
(3) adding 7 parts by weight of modified carbon nano tube, 4 parts by weight of carbon black, 1.2 parts by weight of sulfur and 1.5 parts by weight of antioxidant MB into the double-roll mixing mill in the step (1) in sequence, and mixing for 10min to obtain a mixed rubber material;
(4) injecting the mixed rubber material obtained in the step (3) into a mold, and carrying out hot pressing for 11min under the conditions of the temperature of 152 ℃ and the pressure of 8.5MPa to obtain a primary rubber;
(5) and (4) putting the primary rubber obtained in the step (4) into a flat vulcanizing machine for vulcanization treatment for 44min at the temperature of 180 ℃, and naturally cooling to room temperature to obtain the rubber.
Testing;
and (3) dielectric constant measurement: the method is characterized in that an American Agilent E4980 impedance instrument is adopted for testing, an impedance testing method is adopted for testing the dielectric property, and a test sample with the thickness of 1mm and the area of more than 1 square centimeter is used for testing:
TABLE 1
| Dielectric constant | |
| Example 1 | 9.1 |
| Example 2 | 8.7 |
| Example 3 | 9.6 |
| Control group | 6.5 |
Control group: the difference from the example 1 is that the carbon nanotubes are not modified;
as can be seen from Table 1, the composite material prepared by the present invention has excellent dielectric properties.
And (3) detecting the tearing resistance:
the samples with the same specification of the examples and the comparative examples are detected, and reference is made to GB/T8948;
TABLE 2
| Tear Strength (N/cm) | |
| Example 1 | 226 |
| Example 2 | 235 |
| Example 3 | 255 |
| Comparative example 1 | 178 |
Comparative example 1: the difference from example 3 is that no natural rubber is added.
As can be seen from Table 2, the tear strength was significantly reduced without the addition of natural rubber, and it can be seen that natural rubber and silicone rubber have a significant synergistic effect.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (9)
1. A preparation method of a carbon nano tube/silicon rubber composite material with high dielectric property is characterized by comprising the following steps:
(1) uniformly mixing 60-65 parts by weight of silicone rubber and 10-15 parts by weight of natural rubber, and then adding the mixture into a double-roll mixing roll for mixing for 6-8 min;
(2) uniformly dispersing 10-15 parts by weight of carbon nanotubes into 58-60 parts by weight of ethanol solution, magnetically stirring for 30-35min, adding diphenylsilanediol accounting for 5-6% of the mass of the carbon nanotubes and a coupling agent accounting for 1.2-1.6%, keeping the temperature in a water bath, continuously magnetically stirring for 1-1.2 hours, carrying out suction filtration, and drying to constant weight to obtain modified carbon nanotubes;
(3) sequentially adding 6-8 parts by weight of modified carbon nanotubes, 3-5 parts by weight of carbon black, 1-1.4 parts by weight of sulfur and 1.2-1.6 parts by weight of anti-aging agent into the double-roll mixing mill in the step (1), and mixing for 8-12min to obtain a mixed rubber material;
(4) injecting the mixed rubber material obtained in the step (3) into a mold, and carrying out hot pressing for 10-12min under the conditions that the temperature is 150-;
(5) and (4) putting the primary rubber obtained in the step (4) into a flat vulcanizing machine for vulcanization treatment for 40-50min, and naturally cooling to room temperature to obtain the rubber.
2. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the natural rubber in step (1) is a first-order thin crepe rubber.
3. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the silicone rubber in step (1) is BGP1 silicone rubber.
4. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the ethanol solution in step (2) has a mass fraction of 60%.
5. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the magnetic stirring speed in step (2) is 1200 r/min.
6. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the coupling agent in step (2) is an organosilane coupling agent.
7. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the temperature of the water bath in step (2) is 80 ℃.
8. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the antioxidant in step (3) is antioxidant MB.
9. The method for preparing a carbon nanotube/silicone rubber composite material with high dielectric properties as claimed in claim 1, wherein the vulcanization treatment conditions in step (5) are as follows: the temperature was 180 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114773857A (en) * | 2022-03-28 | 2022-07-22 | 青岛科技大学 | Binary composite silicon rubber material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070904A (en) * | 2010-12-02 | 2011-05-25 | 天津大学 | Silicone rubber composite material and preparation method thereof |
| CN103214707A (en) * | 2013-04-17 | 2013-07-24 | 北京化工大学 | High-dielectric elastomer composite material with low content of carbon nanometer tubes and preparation method of composite material |
| US20170081499A1 (en) * | 2015-09-17 | 2017-03-23 | Shin-Etsu Chemical Co., Ltd. | Silicone rubber composition and power cable |
| CN109135297A (en) * | 2018-08-31 | 2019-01-04 | 安庆市泽烨新材料技术推广服务有限公司 | Silicone rubber for cable sheath material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070904A (en) * | 2010-12-02 | 2011-05-25 | 天津大学 | Silicone rubber composite material and preparation method thereof |
| CN103214707A (en) * | 2013-04-17 | 2013-07-24 | 北京化工大学 | High-dielectric elastomer composite material with low content of carbon nanometer tubes and preparation method of composite material |
| US20170081499A1 (en) * | 2015-09-17 | 2017-03-23 | Shin-Etsu Chemical Co., Ltd. | Silicone rubber composition and power cable |
| CN109135297A (en) * | 2018-08-31 | 2019-01-04 | 安庆市泽烨新材料技术推广服务有限公司 | Silicone rubber for cable sheath material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114773857A (en) * | 2022-03-28 | 2022-07-22 | 青岛科技大学 | Binary composite silicon rubber material and preparation method and application thereof |
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Application publication date: 20200403 |