CN109233288A - A kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement and preparation method thereof - Google Patents
A kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement and preparation method thereof Download PDFInfo
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- CN109233288A CN109233288A CN201811013303.1A CN201811013303A CN109233288A CN 109233288 A CN109233288 A CN 109233288A CN 201811013303 A CN201811013303 A CN 201811013303A CN 109233288 A CN109233288 A CN 109233288A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The present invention discloses a kind of silicon rubber heat-insulating material and preparation method thereof of modified carbon fiber reinforcement, it belongs to heat-insulating material technical field, is prepared by following raw materials: 40~60 parts of methyl vinyl silicone rubber, 40~60 parts of methyl vinyl phenyl silicon rubber, 20~30 parts of white carbon black, 3~10 parts of graphene, 10~15 parts of modified carbon fiber, 0.5~1.5 part of vulcanizing agent.After concentrated nitric acid is handled, the surface roughness of carbon fiber increases carbon fiber in the present invention, and the quantity of oxygen-containing functional group rises；It is impregnated by PEG6000 and α-aminopropyl triethoxysilane, fiber surface has the organo-functional group containing N, Si.Added the silicon rubber of modified carbon fiber, tensile strength has reached 2.96MPa, and elongation at break has reached 57%, compared with the silicon rubber for adding unmodified carbon fiber, tensile strength and elongation at break all greatly improve, and linear ablative rate and mass ablative rate greatly reduce.
Description
Technical field
The present invention relates to heat-insulating material technical field, in particular to a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement
And preparation method thereof.
Background technique
Silicon rubber heat-insulating material is that more insulation layer material is studied and applied to recent domestic, can in ablation process
Dystectic class ceramic layer is formed, with heat-resisting and flame retardant property is good, antioxygenic property is good, anti-small molecule transfer ability is strong, logical
The advantages that strong with property, is expected to that ethylene propylene diene rubber is replaced to become in engine afterburning chamber, is taken the photograph due to thousands of in engine afterburning chamber
The high-speed fuel gas of family name's degree constitutes very big prestige to engine shell bulk structural integrity and assists.Therefore, it is necessary to using heat-insulating material to shell
Carry out pre- thermal protection.
Silicon rubber is that a kind of main chain is Si-O-Si chain, and side chain is the organic polymer of organic substituent (mainly methyl)
Polymer.Silicon rubber mechanical property itself is poor (intensity only has 0.4MPa after pure glue vulcanization), just has practical value after reinforcement.
It is to mention that the fillers such as nanometer calcium carbonate, carbon nanotube, graphene, stannic oxide metal oxide, white carbon black are added in silicon rubber
The effective means of its high performance.Wherein, carbon fiber is due to excellent mechanical property, high temperature resistant, corrosion resistance and electric conductivity
The features such as, it is a kind of preferable reinforced filling of comprehensive performance, but untreated carbon fiber surface is by a large amount of inertia graphite microcrystals
It piles up, so filament surfaces are in polarity, surface can be small, and poor with the wellability of silicone rubber matrix, interface comprehensive performance is poor.This
Outside, high performance carbon fiber surface is smooth, and specific surface area is small, this is but also cannot form effective machinery between fiber and matrix
Anchor cooperation is used, the boundary strength decline between fiber and silicone rubber matrix.
Summary of the invention
The present invention provides silicon rubber heat-insulating materials of a kind of modified carbon fiber reinforcement and preparation method thereof, using carbon modified
Fiber improves the reinforcing effect to silicon rubber.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, is to be prepared by following raw materials: methyl ethylene silicon
40~60 parts of rubber, 40~60 parts of methyl vinyl phenyl silicon rubber, 20~30 parts of white carbon black, 3~10 parts of graphene, carbon modified
10~15 parts of fiber, 0.5~1.5 part of vulcanizing agent；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, in 100 DEG C of water bath with thermostatic control
2h is managed, is subsequently placed in PEG6000 and α-aminopropyl triethoxysilane mixed aqueous solution and impregnates 4h, then clean to neutrality
Drying；The mass fraction of PEG is 2~4% in the mixed aqueous solution, α-aminopropyl triethoxysilane mass fraction is 1
~3%.
Wherein it is preferred to which the mass volume ratio of the carbon fiber and the concentrated nitric acid is 1:40~60g/ml.
Wherein it is preferred to which the vulcanizing agent is 2,5- dimethyl -2,5- bishexane or 2,4- dimethyl 2,4- bishexane.
A kind of preparation method of the silicon rubber heat-insulating material of modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) vulcanizing agent is weighed, is added in step (3) described silicone rubber matrix, is kneaded to uniformly mixed；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein it is preferred to which two sections of vulcanizations are divided into one step cure and post vulcanization, the one step cure is in compression molding
It is carried out on machine, 160 DEG C of curing temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization in air dry oven into
Row, 180 DEG C of curing temperature, pressure is normal pressure, vulcanization time 2h.
Beneficial effects of the present invention:
Carbon fiber in the present invention is after concentrated nitric acid is handled, and the surface roughness of carbon fiber increases, the number of oxygen-containing functional group
Amount rises；It is impregnated by PEG6000 and α-aminopropyl triethoxysilane, fiber surface has the organo-functional group containing N, Si.
The silicon rubber of modified carbon fiber was added, tensile strength has reached 2.96MPa, and elongation at break has reached 57%, not with addition
The silicon rubber of modified carbon fiber is compared, and tensile strength and elongation at break all greatly improve, linear ablative rate and mass ablative rate
Greatly reduce.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is prepared by following raw materials:
50 parts of methyl vinyl silicone rubber, 50 parts of methyl vinyl phenyl silicon rubber, 25 parts of white carbon black, 6 parts of graphene, modified carbon fiber
12 parts, vulcanizing agent 2,1.0 parts of 5- dimethyl -2,5- bishexane；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, carbon fiber and the concentrated nitric acid
Mass volume ratio is 1:50g/ml；2h is handled in 100 DEG C of water bath with thermostatic control, is subsequently placed in three second of PEG6000 and α-aminopropyl
4h is impregnated in the mixed aqueous solution of oxysilane, then cleans to neutral drying；The mass fraction of PEG in the mixed aqueous solution
It is 2% for 3%, α-aminopropyl triethoxysilane mass fraction.
The preparation method of the silicon rubber heat-insulating material of the present embodiment modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) weighing vulcanizing agent is 2,5- dimethyl -2,5- bishexane, is added in step (3) described silicone rubber matrix, is kneaded
Extremely it is uniformly mixed；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein, two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, sulphur
Change 160 DEG C of temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization carries out in air dry oven, curing temperature
180 DEG C, pressure is normal pressure, vulcanization time 2h.
Embodiment 2
The present embodiment provides a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is prepared by following raw materials:
40 parts of methyl vinyl silicone rubber, 60 parts of methyl vinyl phenyl silicon rubber, 20 parts of white carbon black, 10 parts of graphene, modified carbon fiber
Tie up 10 parts, vulcanizing agent 2,1.5 parts of 5- dimethyl -2,5- bishexane；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, carbon fiber and the concentrated nitric acid
Mass volume ratio is 1:40g/ml；2h is handled in 100 DEG C of water bath with thermostatic control, is subsequently placed in three second of PEG6000 and α-aminopropyl
4h is impregnated in the mixed aqueous solution of oxysilane, then cleans to neutral drying；The mass fraction of PEG in the mixed aqueous solution
It is 1% for 4%, α-aminopropyl triethoxysilane mass fraction.
The preparation method of the silicon rubber heat-insulating material of the present embodiment modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) weighing vulcanizing agent is 2,5- dimethyl -2,5- bishexane, is added in step (3) described silicone rubber matrix, is kneaded
Extremely it is uniformly mixed；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein, two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, sulphur
Change 160 DEG C of temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization carries out in air dry oven, curing temperature
180 DEG C, pressure is normal pressure, vulcanization time 2h.
Embodiment 3
The present embodiment provides a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is prepared by following raw materials:
60 parts of methyl vinyl silicone rubber, 40 parts of methyl vinyl phenyl silicon rubber, 30 parts of white carbon black, 3 parts of graphene, modified carbon fiber
15 parts, 2,4- dimethyl 2,0.5 part of 4- bishexane；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, carbon fiber and the concentrated nitric acid
Mass volume ratio is 1:60g/ml；2h is handled in 100 DEG C of water bath with thermostatic control, is subsequently placed in three second of PEG6000 and α-aminopropyl
4h is impregnated in the mixed aqueous solution of oxysilane, then cleans to neutral drying；The mass fraction of PEG in the mixed aqueous solution
It is 3% for 2%, α-aminopropyl triethoxysilane mass fraction.
The preparation method of the silicon rubber heat-insulating material of the present embodiment modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) 2,4- dimethyl 2 is weighed, 4- bishexane is added in step (3) described silicone rubber matrix, is kneaded equal to mixing
It is even；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein, two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, sulphur
Change 160 DEG C of temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization carries out in air dry oven, curing temperature
180 DEG C, pressure is normal pressure, vulcanization time 2h.
Embodiment 4
The present embodiment provides a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is prepared by following raw materials:
45 parts of methyl vinyl silicone rubber, 55 parts of methyl vinyl phenyl silicon rubber, 22 parts of white carbon black, 8 parts of graphene, modified carbon fiber
14 parts, 2,4- dimethyl 2,1.2 parts of 4- bishexane；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, carbon fiber and the concentrated nitric acid
Mass volume ratio is 1:45g/ml；2h is handled in 100 DEG C of water bath with thermostatic control, is subsequently placed in three second of PEG6000 and α-aminopropyl
4h is impregnated in the mixed aqueous solution of oxysilane, then cleans to neutral drying；The mass fraction of PEG in the mixed aqueous solution
It is 2.5% for 3.5%, α-aminopropyl triethoxysilane mass fraction.
The preparation method of the silicon rubber heat-insulating material of the present embodiment modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) 2,4- dimethyl 2 is weighed, 4- bishexane is added in step (3) described silicone rubber matrix, is kneaded equal to mixing
It is even；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein, two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, sulphur
Change 160 DEG C of temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization carries out in air dry oven, curing temperature
180 DEG C, pressure is normal pressure, vulcanization time 2h.
Embodiment 5
The present embodiment provides a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is prepared by following raw materials:
55 parts of methyl vinyl silicone rubber, 45 parts of methyl vinyl phenyl silicon rubber, 28 parts of white carbon black, 4 parts of graphene, modified carbon fiber
12 parts, 1.2 parts of 2,5- dimethyl -2,5- bishexane；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, carbon fiber and the concentrated nitric acid
Mass volume ratio is 1:55g/ml；2h is handled in 100 DEG C of water bath with thermostatic control, is subsequently placed in three second of PEG6000 and α-aminopropyl
4h is impregnated in the mixed aqueous solution of oxysilane, then cleans to neutral drying；The mass fraction of PEG in the mixed aqueous solution
It is 2% for 3%, α-aminopropyl triethoxysilane mass fraction.
The preparation method of the silicon rubber heat-insulating material of the present embodiment modified carbon fiber reinforcement, includes the following steps:
(1) weigh methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber, be added in kneading machine be kneaded to
Pellucidity prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded to mixing
Uniformly；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) 2,5- dimethyl -2,5- bishexane is weighed, is added in step (3) described silicone rubber matrix, is kneaded equal to mixing
It is even；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
Wherein, two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, sulphur
Change 160 DEG C of temperature, pressure 10MPa, vulcanization time 15min；The post vulcanization carries out in air dry oven, curing temperature
180 DEG C, pressure is normal pressure, vulcanization time 2h.
Performance test, the ablation resistance of above-described embodiment by ablator ablative test method (GJB 323A/96) into
Row measurement.According to " test (GB/T 528-1998) of vulcanized rubber or thermoplastic elastomer tensile stress-strain performance ", measurement is flat
The tensile strength and fracture elongation of row slice direction and vertical slice direction sample.According to the measurement (GB/ of vulcanized rubber density
T533-91 density measurement) is carried out.Shown in the performance test results following table:
1 the performance test results table of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement, it is characterised in that be to be prepared by following raw materials: methyl
40~60 parts of vinylsiloxane rubber, 40~60 parts of methyl vinyl phenyl silicon rubber, 20~30 parts of white carbon black, graphene 3~10
Part, 10~15 parts of modified carbon fiber, 0.5~1.5 part of vulcanizing agent；
The preparation method of the modified carbon fiber is: carbon fiber being placed in concentrated nitric acid, is handled in 100 DEG C of water bath with thermostatic control
2h is subsequently placed in PEG6000 and α-aminopropyl triethoxysilane mixed aqueous solution and impregnates 4h, then cleans to neutral baking
It is dry；In the mixed aqueous solution mass fraction of PEG be 2~4%, α-aminopropyl triethoxysilane mass fraction be 1~
3%.
2. a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement according to claim 1, it is characterised in that: the carbon
The mass volume ratio of fiber and the concentrated nitric acid is 1:40~60g/ml.
3. a kind of silicon rubber heat-insulating material of modified carbon fiber reinforcement according to claim 1, it is characterised in that: the sulphur
Agent is 2,5- dimethyl -2,5- bishexane or 2,4- dimethyl 2,4- bishexane.
4. a kind of preparation method of the silicon rubber heat-insulating material of the described in any item modified carbon fiber reinforcement of claims 1 to 3,
It is characterized in that including the following steps:
(1) methyl vinyl silicone rubber and methyl vinyl phenyl silicon rubber are weighed, is added in kneading machine and is kneaded to transparent
State prepares silicone rubber matrix；
(2) it weighs modified white carbon black and chopped carbon fiber is added in the silicone rubber matrix that step (1) obtains, be kneaded equal to mixing
It is even；
(3) graphene is weighed, is added in silicone rubber matrix obtained in step (2), is kneaded to uniformly mixed；
(4) vulcanizing agent is weighed, is added in step (3) described silicone rubber matrix, is kneaded to uniformly mixed；
(5) grind the film of required thickness out and shape using open mill, carry out two sections of vulcanizations to get.
5. a kind of preparation method of the silicon rubber heat-insulating material of modified carbon fiber reinforcement according to claim 4, feature
Be: two sections of vulcanizations are divided into one step cure and post vulcanization, and the one step cure carries out on vulcanizing press, vulcanization temperature
160 DEG C, pressure 10MPa, vulcanization time 15min of degree；The post vulcanization carries out in air dry oven, and 180 DEG C of curing temperature,
Pressure is normal pressure, vulcanization time 2h.
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Cited By (4)
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| CN110669343A (en) * | 2019-10-24 | 2020-01-10 | 广州赫尔普化工有限公司 | Wear-resistant heat-conducting silicone rubber composite material and preparation method thereof |
| CN111312444A (en) * | 2019-12-18 | 2020-06-19 | 长沙华脉新材料有限公司 | High-temperature-resistant anti-corrosion cable |
| CN113502019A (en) * | 2021-07-26 | 2021-10-15 | 苏州润佳高分子材料有限公司 | Low-odor soft touch material and preparation method thereof |
| CN116715960A (en) * | 2023-06-07 | 2023-09-08 | 昆山力普电子橡胶有限公司 | Mobile storage network hard disk protective sleeve and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669343A (en) * | 2019-10-24 | 2020-01-10 | 广州赫尔普化工有限公司 | Wear-resistant heat-conducting silicone rubber composite material and preparation method thereof |
| CN111312444A (en) * | 2019-12-18 | 2020-06-19 | 长沙华脉新材料有限公司 | High-temperature-resistant anti-corrosion cable |
| CN113502019A (en) * | 2021-07-26 | 2021-10-15 | 苏州润佳高分子材料有限公司 | Low-odor soft touch material and preparation method thereof |
| CN116715960A (en) * | 2023-06-07 | 2023-09-08 | 昆山力普电子橡胶有限公司 | Mobile storage network hard disk protective sleeve and preparation method thereof |
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Application publication date: 20190118 |