CN108467589A - A kind of Silicone Rubber Modified by Carbon Nanotubes material - Google Patents
A kind of Silicone Rubber Modified by Carbon Nanotubes material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a kind of Silicone Rubber Modified by Carbon Nanotubes material, raw material includes：Silicon rubber, polyaspartic ester, ethylene-acrylate rubber, aerosil, carbon nanotube, ferric oxalate, montmorillonite, galapectite, vinal, glass fibre, zinc oxide, silane coupling agent, 2; 5 dimethyl 2; 5 two (t-butylperoxy) hexanes, benzoyl peroxide, altax, N; 1,2 propane diamine of the bis- sub- bigcatkin willows of N', N methylols 3 (dimethoxy phosphono) propionamide.Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, heat-resist, ageing-resistant and excellent fireproof performance, intensity are high.
Description
Technical field
The present invention relates to silastic material technical field more particularly to a kind of Silicone Rubber Modified by Carbon Nanotubes materials.
Background technology
Silicon rubber is that the one of the organic groups such as methyl, ethyl, phenyl are connected on Si atoms using Si-O inorganic structures as main chain
Half inorganic polymer of kind, with excellent resistance to low temperature, excellent dielectric properties, good resistance to elemental oxygen, ozone attack
Effect and radiation resistance, low surface energy and physiological inertia, highly-breathable have been widely used in Aeronautics and Astronautics, outer at present
Add the fields such as agent, electromagnetic shielding, membrane material, electric, medicine, daily necessities, and has become indispensable in national economy
A kind of elastomeric material.With the development of society, more stringent requirements are proposed for performance of the people to silicon rubber, especially for answering
Silicon rubber material for the high-end smart pointed collar domain such as aerospace, nuclear power equipment and national defense safety has higher requirement, existing
Silastic material be applied in aerospace, nuclear power equipment and the high-end smart pointed collar domain such as national defense safety, there are still heat resistance,
Resistance to ag(e)ing and the not good enough defect of flame retardant property, limit its application.
Invention content
Technical problems based on background technology, the present invention propose a kind of Silicone Rubber Modified by Carbon Nanotubes material,
It is heat-resist, ageing-resistant and excellent fireproof performance, intensity height.
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：Silicon rubber 80-95
Part, 5-20 parts of polyaspartic ester, 3-8 parts of ethylene-acrylate rubber, 2-10 parts of aerosil, carbon nanotube
5-17 parts, 2-9 parts of ferric oxalate, 2-10 parts of montmorillonite, 1-8 parts of galapectite, 1-3.8 parts of vinal, glass fibre 2-3.5
Part, 1-3.8 parts of zinc oxide, 0.5-1.3 parts of silane coupling agent, two (t-butylperoxy) hexane 0.1- of 2,5- dimethyl -2,5-
0.5 part, 0.05-0.35 parts of benzoyl peroxide, 0.1-0.22 parts of altax, N, the bis- sub- bigcatkin willow -1,2- propane diamine 1- of N'-
3.8 parts, 3-9 parts of N- methylols -3- (dimethoxy phosphono) propionamide.
Preferably, the carbon nanotube is modified carbon nano-tube；The modified carbon nano-tube is according to following technique system
It is standby：Acidification carbon nanotube is added in dimethyl sulfoxide (DMSO), N is added after ultrasonic disperse, N '-carbonyl dimidazoles are warming up to 65-75
DEG C, 5-8h is stirred, amino list is then added and blocks dimethyl silicone polymer, 15-20h, reaction knot are stirred to react at 55-65 DEG C
It is filtered, washed, dries after beam, acetone extraction 25-35h is then used at 65-75 DEG C, material A is obtained after dry；By material A, receive
Rice iron oxide, nano cupric oxide and nano tin dioxide are added in absolute ethyl alcohol, ultrasound 5-10h after being warming up to 60-75 DEG C, filtering,
It washs, be dried to obtain the modified carbon nano-tube.
Preferably, in the preparation process of modified carbon nano-tube, acidification carbon nanotube, N, N '-carbonyl dimidazoles, amino list
The weight ratio for blocking dimethyl silicone polymer is 3-8：0.3-0.5：6-11.
Preferably, in the preparation process of modified carbon nano-tube, material A, nano-sized iron oxide, nano cupric oxide, nano oxygen
The weight ratio for changing tin is 5-13：2-5：1-4：3-8.
Preferably, the montmorillonite is the montmorillonite that dioctadecyl dimethyl ammonium chloride is modified.
Preferably, the galapectite is the galapectite that vinyltrimethoxysilane is modified.
Preferably, the silane coupling agent is silane coupling agent KH-560, Silane coupling reagent KH-570, silane coupling agent
The mixture of one or more of KH-580, silane coupling A -171.
Silicone Rubber Modified by Carbon Nanotubes material of the present invention using silicon rubber as major ingredient, while adding poly- lucid asparagus
Propylhomoserin ester, ethylene-acrylate rubber and its coordinate, improve the compatibility of system, three made to play best synergistic effect,
Under the premise of keeping lower cost, significantly improve the heat-resistant stable of rubber material, tensile strength, tearing strength,
Oil resistivity, resistance to ag(e)ing and elasticity；In the preparation process of preferred embodiment modified carbon nano-tube, first to be acidified carbon nanotube and N,
N '-carbonyl dimidazoles are raw material makes the carboxyl and N of acidification carbon nano tube surface, N '-carbonyls two by controlling the condition of reaction
Imidazoles nitrogen in imidazoles is reacted, after amino list sealing end dimethyl silicone polymer is added, remaining in N '-carbonyl dimidazoles
The amino that blocks in dimethyl silicone polymer of imidazoles nitrogen and amino list further reacted, it is poly- to block amino list
Dimethyl siloxane has successfully been grafted to the surface of carbon nanotube, has obtained material A；By material A, nano-sized iron oxide, nano oxygen
After changing copper and nano tin dioxide mixing, the amino list sealing end dimethyl silicone polymer on material A surface can be with nano-sized iron oxide, nanometer
Copper oxide and nano tin dioxide effect, have obtained modified carbon nano-tube, have been added into system, be uniformly dispersed in system, and one
Aerosil, ferric oxalate, montmorillonite, galapectite, vinal, glass fibre, N in aspect, with system,
Bis- sub- bigcatkin willow -1, the 2- propane diamine cooperations of N'-, can capture the free radical generated during silicon rubber thermo-oxidative ageing, hence it is evident that reduce side
The generation of methyl oxidation product assigns material excellent thermal stability, slows down the aging of rubber material, it is excellent to assign rubber material
Different resistance to ag(e)ing on the other hand can be with the montmorillonite in system, galapectite, N- methylols -3- (dimethoxy phosphono) third
Amide coordinates, and the residue densification consolidation, heat rejection effect after rubber material can be made to burn are good, and carbon yield is high, heat release rate drop
It is low, assign rubber material excellent anti-flammability；With 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, benzoyl peroxide first
Acyl is vulcanizing agent, while adding altax cooperation, hence it is evident that the time of scorch and sulfurizing time for shortening Blend rubber significantly carry
The high mechanical property of material, heat resistance and Compression Set.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：95 parts of silicon rubber,
5 parts of polyaspartic ester, 8 parts of ethylene-acrylate rubber, 2 parts of aerosil, 17 parts of carbon nanotube, ferric oxalate 2
Part, 10 parts of montmorillonite, 1 part of galapectite, 3.8 parts of vinal, 2 parts of glass fibre, 3.8 parts of zinc oxide, silane coupling agent
0.5 part, 0.5 part of 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 0.05 part of benzoyl peroxide, altax
0.22 part, N, bis- 1 part of the Asia bigcatkin willow -1,2- propane diamine of N'-, 9 parts of N- methylols -3- (dimethoxy phosphono) propionamide.
Embodiment 2
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：80 parts of silicon rubber,
20 parts of polyaspartic ester, 3 parts of ethylene-acrylate rubber, 10 parts of aerosil, 5 parts of carbon nanotube, ferric oxalate
9 parts, 2 parts of montmorillonite, 8 parts of galapectite, 1 part of vinal, 3.5 parts of glass fibre, 1 part of zinc oxide, silane coupling agent 1.3
Part, 0.1 part of 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 0.35 part of benzoyl peroxide, altax 0.1
Part, N, bis- 3.8 parts of the Asia bigcatkin willow -1,2- propane diamine of N'-, 3 parts of N- methylols -3- (dimethoxy phosphono) propionamide.
Embodiment 3
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：92 parts of silicon rubber,
7 parts of polyaspartic ester, 7.2 parts of ethylene-acrylate rubber, 3.6 parts of aerosil, 14 parts of carbon nanotube, grass
3.6 parts of sour iron, 8 parts of montmorillonite, 1.9 parts of galapectite, 3.6 parts of vinal, 2.5 parts of glass fibre, 3.2 parts of zinc oxide,
0.6 part of silane coupling agent, 0.42 part of 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 0.1 part of benzoyl peroxide,
0.2 part of altax, N, bis- 1.3 parts of the Asia bigcatkin willow -1,2- propane diamine of N'-, N- methylols -3- (dimethoxy phosphono) propionyl
8.3 parts of amine；
Wherein, the carbon nanotube is modified carbon nano-tube；The modified carbon nano-tube is prepared according to following technique：
Acidification carbon nanotube is added in dimethyl sulfoxide (DMSO), N is added after ultrasonic disperse, N '-carbonyl dimidazoles are warming up to 65 DEG C, stirring
Then 8h is added amino list and blocks dimethyl silicone polymer, wherein acidification carbon nanotube, N, N '-carbonyl dimidazoles, amino list
The weight ratio for blocking dimethyl silicone polymer is 3：0.5：6,20h is stirred to react at 55 DEG C, be filtered, washed after reaction,
It is dry, acetone extraction 35h is then used at 65 DEG C, and material A is obtained after dry；By material A, nano-sized iron oxide, nano cupric oxide
It is added in absolute ethyl alcohol with nano tin dioxide, wherein material A, the weight of nano-sized iron oxide, nano cupric oxide, nano tin dioxide
Than being 13：2：4：3, ultrasound 10h after being warming up to 60 DEG C are filtered, washed, are dried to obtain the modified carbon nano-tube；
The montmorillonite is the montmorillonite that dioctadecyl dimethyl ammonium chloride is modified；
The galapectite is the galapectite that vinyltrimethoxysilane is modified；
The silane coupling agent is silane coupling agent KH-560.
Embodiment 4
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：86 parts of silicon rubber,
15 parts of polyaspartic ester, 4.6 parts of ethylene-acrylate rubber, 8 parts of aerosil, 8 parts of carbon nanotube, oxalic acid
8 parts of iron, 4 parts of montmorillonite, 7.1 parts of galapectite, 1.3 parts of vinal, 3.2 parts of glass fibre, 1.5 parts of zinc oxide, silane
1 part of coupling agent, 0.18 part of 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 0.3 part of benzoyl peroxide, accelerating agent
0.12 part of DM, N, bis- 3.2 parts of the Asia bigcatkin willow -1,2- propane diamine of N'-, N- methylols -3- (dimethoxy phosphono) propionamide 4.2
Part；
Wherein, the carbon nanotube is modified carbon nano-tube；The modified carbon nano-tube is prepared according to following technique：
Acidification carbon nanotube is added in dimethyl sulfoxide (DMSO), N is added after ultrasonic disperse, N '-carbonyl dimidazoles are warming up to 75 DEG C, stirring
Then 5h is added amino list and blocks dimethyl silicone polymer, wherein acidification carbon nanotube, N, N '-carbonyl dimidazoles, amino list
The weight ratio for blocking dimethyl silicone polymer is 8：0.3：11,15h is stirred to react at 65 DEG C, be filtered, washed after reaction,
It is dry, acetone extraction 25h is then used at 75 DEG C, and material A is obtained after dry；By material A, nano-sized iron oxide, nano cupric oxide
It is added in absolute ethyl alcohol with nano tin dioxide, wherein material A, the weight of nano-sized iron oxide, nano cupric oxide, nano tin dioxide
Than being 5：5：1:8, ultrasound 5h after being warming up to 75 DEG C are filtered, washed, are dried to obtain the modified carbon nano-tube；
The montmorillonite is the montmorillonite that dioctadecyl dimethyl ammonium chloride is modified；
The galapectite is the galapectite that vinyltrimethoxysilane is modified；
The silane coupling agent is Silane coupling reagent KH-570.
Embodiment 5
A kind of Silicone Rubber Modified by Carbon Nanotubes material proposed by the present invention, raw material include by weight：90 parts of silicon rubber,
16 parts of polyaspartic ester, 6 parts of ethylene-acrylate rubber, 7 parts of aerosil, 12 parts of carbon nanotube, ferric oxalate
6 parts, it is 5 parts of montmorillonite, 4 parts of galapectite, 3.2 parts of vinal, 2.8 parts of glass fibre, 1.9 parts of zinc oxide, silane coupled
1 part of agent, 0.35 part of 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 0.3 part of benzoyl peroxide, altax
0.16 part, N, bis- 2.3 parts of the Asia bigcatkin willow -1,2- propane diamine of N'-, 6 parts of N- methylols -3- (dimethoxy phosphono) propionamide；
Wherein, the carbon nanotube is modified carbon nano-tube；The modified carbon nano-tube is prepared according to following technique：
Acidification carbon nanotube is added in dimethyl sulfoxide (DMSO), N is added after ultrasonic disperse, N '-carbonyl dimidazoles are warming up to 70 DEG C, stirring
Then 6h is added amino list and blocks dimethyl silicone polymer, 17h is stirred to react at 60 DEG C, be filtered, washed after reaction,
It is dry, acetone extraction 30h is then used at 70 DEG C, and material A is obtained after dry；By material A, nano-sized iron oxide, nano cupric oxide
It is added in absolute ethyl alcohol with nano tin dioxide, ultrasound 8h after being warming up to 68 DEG C, is filtered, washed, is dried to obtain the carbon modified and receives
Mitron；
In the preparation process of modified carbon nano-tube, acidification carbon nanotube, N, N '-carbonyl dimidazoles, amino list sealing end are poly-
The weight ratio of dimethyl siloxane is 7：0.4：9；
In the preparation process of modified carbon nano-tube, material A, nano-sized iron oxide, nano cupric oxide, nano tin dioxide weight
Amount is than being 9：4：3：5；
The montmorillonite is the montmorillonite that dioctadecyl dimethyl ammonium chloride is modified；
The galapectite is the galapectite that vinyltrimethoxysilane is modified；
The silane coupling agent is silane coupling agent KH-560, Silane coupling reagent KH-570, silane coupling agent KH-580, silicon
The mixture of alkane coupling agent A-171, and silane coupling agent KH-560, Silane coupling reagent KH-570, silane coupling agent KH-580, silicon
The weight ratio of alkane coupling agent A-171 is 3：4：6：5.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of Silicone Rubber Modified by Carbon Nanotubes material, which is characterized in that its raw material includes by weight：80-95 parts of silicon rubber,
5-20 parts of polyaspartic ester, 3-8 parts of ethylene-acrylate rubber, 2-10 parts of aerosil, carbon nanotube 5-17
Part, 2-9 parts of ferric oxalate, 2-10 parts of montmorillonite, 1-8 parts of galapectite, 1-3.8 parts of vinal, 2-3.5 parts of glass fibre,
1-3.8 parts of zinc oxide, 0.5-1.3 parts of silane coupling agent, two (t-butylperoxy) hexane 0.1-0.5 of 2,5- dimethyl -2,5-
Part, 0.05-0.35 parts of benzoyl peroxide, 0.1-0.22 parts of altax, N, the bis- sub- bigcatkin willow -1,2- propane diamine 1-3.8 of N'-
Part, 3-9 parts of N- methylols -3- (dimethoxy phosphono) propionamide.
2. Silicone Rubber Modified by Carbon Nanotubes material according to claim 1, which is characterized in that the carbon nanotube is carbon modified
Nanotube；The modified carbon nano-tube is prepared according to following technique：Acidification carbon nanotube is added in dimethyl sulfoxide (DMSO), is surpassed
N is added after sound dispersion, N '-carbonyl dimidazoles are warming up to 65-75 DEG C, stir 5-8h, and amino list is then added and blocks poly dimethyl
Siloxanes is stirred to react 15-20h at 55-65 DEG C, is filtered, washed, dries after reaction, then with third at 65-75 DEG C
Ketone extracts 25-35h, and material A is obtained after dry；Nothing is added in material A, nano-sized iron oxide, nano cupric oxide and nano tin dioxide
In water-ethanol, ultrasound 5-10h after being warming up to 60-75 DEG C is filtered, washed, is dried to obtain the modified carbon nano-tube.
3. Silicone Rubber Modified by Carbon Nanotubes material according to claim 2, which is characterized in that in the preparation of modified carbon nano-tube
In the process, it is acidified carbon nanotube, N, the weight ratio that N '-carbonyl dimidazoles, amino list block dimethyl silicone polymer is 3-8：
0.3-0.5：6-11.
4. according to Silicone Rubber Modified by Carbon Nanotubes material described in Claims 2 or 3, which is characterized in that in modified carbon nano-tube
In preparation process, material A, nano-sized iron oxide, nano cupric oxide, nano tin dioxide weight ratio be 5-13：2-5：1-4：3-8.
5. according to any one of the claim 1-4 Silicone Rubber Modified by Carbon Nanotubes materials, which is characterized in that the montmorillonite
The montmorillonite being modified for dioctadecyl dimethyl ammonium chloride.
6. according to any one of the claim 1-5 Silicone Rubber Modified by Carbon Nanotubes materials, which is characterized in that the galapectite
The galapectite being modified for vinyltrimethoxysilane.
7. according to any one of the claim 1-6 Silicone Rubber Modified by Carbon Nanotubes materials, which is characterized in that the silane is even
Connection agent is in silane coupling agent KH-560, Silane coupling reagent KH-570, silane coupling agent KH-580, silane coupling A -171
One or more kinds of mixtures.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370266A (en) * | 2018-10-15 | 2019-02-22 | 吉林师范大学 | A kind of modified carbon nano-tube and its preparation method and application |
| CN116041959A (en) * | 2022-12-13 | 2023-05-02 | 无锡海特新材料研究院有限公司 | High dielectric constant silicon rubber and preparation method thereof |
-
2018
- 2018-03-30 CN CN201810293726.7A patent/CN108467589A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370266A (en) * | 2018-10-15 | 2019-02-22 | 吉林师范大学 | A kind of modified carbon nano-tube and its preparation method and application |
| CN116041959A (en) * | 2022-12-13 | 2023-05-02 | 无锡海特新材料研究院有限公司 | High dielectric constant silicon rubber and preparation method thereof |
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