CN108384129A - A kind of resistance to ablation EPDM rubber insulation of polyhedral oligomeric silsesquioxane filling - Google Patents
A kind of resistance to ablation EPDM rubber insulation of polyhedral oligomeric silsesquioxane filling Download PDFInfo
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- CN108384129A CN108384129A CN201810315485.1A CN201810315485A CN108384129A CN 108384129 A CN108384129 A CN 108384129A CN 201810315485 A CN201810315485 A CN 201810315485A CN 108384129 A CN108384129 A CN 108384129A
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four 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 polyhedral oligomeric silsesquioxanes (POSS) to fill the ethylene propylene diene rubber of resistance to ablation (EPDM) heat insulation layer, it is 60~85 parts of ethylene propylene diene rubber that it, which forms (mass parts), 15~40 parts of neoprene, 15~25 parts of reinforcing agent, 6~15 parts of organic fiber, 20~30 parts of fire resistant resin, 25~35 parts of high temperature resistant POSS, 8~40 parts of modifying agent, 5~8 parts of metal oxide, 4 parts of vulcanizing agent, 2 parts of stearic acid.The present invention realizes graft modifications of the POSS on EPDM rubber base material using POSS modifying agent, add the excellent POSS of high temperature resistance, reinforcing agent, resin and organic fiber simultaneously, significantly improve the ablation resistance of EPDM heat insulation layers, product ablation resistance is excellent, suitable for requiring the thermal protection field of high temperature resistant ablation, the thermal protection technology field especially suitable for solid propellant rocket.
Description
Technical field
The present invention relates to ablation resistant material technical field, specifically a kind of polyhedral oligomeric silsesquioxane (POSS) filling
The ethylene propylene diene rubber of resistance to ablation (EPDM) heat insulation layer.
Background technology
EPDM (EPDM) heat-insulating material mainly mixes fire retardant, fiber and inorganic filler etc. by matrix of EPDM rubber
Auxiliary agent has the characteristics that low, ageing-resistant, the resistance to ablation of density, good heat-proof quality and excellent mechanical property, thus as solid
Rocket engine internal insulation is widely applied.But strategy of new generation, tactical missile more it is prominent at high speed, high-precision,
Height existence and high reliability, this requires the height that EPDM heat insulation layers cope with missile armament with higher ablation resistance is prominent anti-
Property and high maneuverability.
Polyhedral oligomeric silsesquioxane (POSS) is a kind of novel organic-inorganic materials, has structure
The excellent characteristic such as designability, high thermal stability and anti-flammability, nanometer size effect and good dissolubility.It can replace
The common fire retardant such as the ammonium polyphosphate in heat insulation layer, decabromodiphenyl oxide at present, at the same can with modified silicone resin, pbo fiber and
EPDM rubber etc., due to its special cage modle Si-O structure, being formed in ablation process can porcelain layer, effectively reduction heat insulation layer burning
Erosion rate improves heat insulation layer comprehensive performance.
The He Jiyu of Beijing Institute of Technology is contained by the way that polyphosphoric acid amine and ladder-like poly-phenyl silsesquioxane and the two is added
The optimization of amount, so as to get EPDM rubber material achieve the effect that low fever's erosion and its good mechanical properties, and applied for patent
201010606018.8, but this report has pertained only to a kind of inertia polyhedral oligomeric silsesquioxane, as fire retardant, and
Carbonization degree is in 0.13~0.17mm/s.
Current existing EPDM heat insulation layers have certain ablation resistance, oxyacetylene ablation rate substantially 0.08~
0.20mm/s cannot be satisfied the patience ablation property requirement of novel high overload and high maneuverability energy engine calls.
Invention content
The technical problem to be solved by the present invention is to cannot be satisfied high overload and high maneuverability energy for existing EPDM heat insulation layers
The prior art of engine calls is insufficient, and it is adiabatic to provide a kind of polyhedral oligomeric silsesquioxane (POSS) filling EPDM of resistance to ablation
Layer, the heat insulation layer have excellent ablation resistance, can meet high overload and high maneuverability energy engine calls.
In order to solve the above technical problems, the present invention provides following technical scheme：A kind of polyhedral oligomeric silsesquioxane
(POSS) EPDM of resistance to ablation heat insulation layers are filled, are made of the component of following mass parts：
Further, the Third monomer of above-mentioned ethylene propylene diene rubber is ethylidene norbornene, ethylidene in ethylene propylene diene rubber
The content of norbornene is 5.0%-12.0%, the content of ethylene is 53.0%~59.0%.
Further, above-mentioned neoprene is non-sulfur-modified neoprene.
Further, above-mentioned reinforcing agent be carbon nanotube, carbon nano-fiber, carbon black and white carbon in one kind or they
Mixed system.
Further, above-mentioned organic fiber is Fanglun 1414 (PPTA), polysulphonamide fiber
(PSA), one kind or their mixture in Poly-p-phenylene benzobisthiazole (PBO), polyacrylonitrile fibre (PAN) etc.
System.
Further, above-mentioned fire resistant resin be one kind in silicones, phenolic resin, polyimide resin etc. or they
Mixed system.
Further, above-mentioned high temperature resistant POSS is trapezoidal phenyl oligomeric silsesquioxane, octaphenyl polyhedral oligomeric sesquialter silicon
Oxygen alkane and phosphorous polyhedral oligomeric silsesquioxane and one kind in other high temperature resistant polyhedral oligomeric silsesquioxane compounds or
Their mixed system；
Further, above-mentioned modifying agent is mono-vinyl polyhedral oligomeric silsesquioxane, bi-vinyl polyhedral oligomeric sesquialter
Siloxanes, tetravinyl polyhedral oligomeric silsesquioxane, eight ethenyl cage model oligomeric silsesquioxanes, phenyl vinyl cage modle are low
The polyhedral oligomeric of polysilsesquioxane, isobutyl vinyl ether-glycidyl polyhedral oligomeric silsesquioxane and other carbon-carbon double bonds groups times
Half siloxanes；
Further, above-mentioned metal oxide is one kind or their mixed system in magnesia and zinc oxide.
Further, above-mentioned crosslinking agent be cumyl peroxide, 2,5- dimethyl -2,5- diperoxies benzene methyl oneself
Alkane, di-tert-butyl peroxide, 2,5- dimethyl -2,5- dual-tert-butyl peroxies hexane, 2,5- dimethyl -2,5- dual-tert-butyls
Peroxy -3- hexins, benzoyl peroxide, Isosorbide-5-Nitrae-dual-tert-butyl peroxy isopropyl base benzene, 1,1- dual-tert-butyl peroxides butylcyclohexane,
1,1- di-t-butyl peroxy -3,3,5- trimethyl-cyclohexanes and one kind in other organic peroxide vulcanizing agents or they
Mixed system.
Further, above-mentioned stearic acid is commercially available general stearic acid.
The present invention is by research shows that ethenyl cage model oligomeric silsesquioxane, phenyl vinyl polyhedral oligomeric sesquialter silicon
Oxygen alkane, isobutyl vinyl ether-glycidyl polyhedral oligomeric silsesquioxane and other carbon-carbon double bonds group isoreactivity polyhedral oligomeric sesquialter silicon
Oxygen alkane can be at high temperature grafted to by peroxide initiator on EPDM rubber strand, and notable modified epdm rubber heat is steady
Qualitatively on the basis of, be further introduced into high temperature resistant polyhedral oligomeric silsesquioxane, fire resistant resin and high temperature resistant reinforcing agent and
High-temperature fibre realizes that the ablation resistance of EPDM rubber improves.
The present invention realizes graft modifications of the POSS on EPDM rubber base material using POSS modifying agent, while adding high temperature resistant
POSS, reinforcing agent, resin and the organic fiber haveing excellent performance, significantly improve the ablation resistance of EPDM heat insulation layers.Polyhedron is low
Polysilsesquioxane (POSS) the filling EPDM of resistance to ablation heat insulation layer ablation resistances are excellent, suitable for requiring the heat of high temperature resistant ablation
Protection field, the thermal protection technology field especially suitable for solid propellant rocket.
The present invention has an advantageous effect in that compared with existing current EPDM heat insulation layers：
1, the ablation resistance of EPDM heat insulation layers of the present invention is significantly improved compared with the prior art；
2, charring layer is complete, fine and close after EPDM insulation erosions of the present invention.
Description of the drawings
Fig. 1 is pattern photo of the sample of the embodiment of the present invention after oxyacetylene ablation；
Fig. 2 is pattern photo of the comparative example sample of the present invention after oxyacetylene ablation.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, right below in conjunction with drawings and examples
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Note：It is mass parts that the deal illustrated is not done in embodiment.
Embodiment 1
Sequentially added in 25 DEG C of two-roll mills 80 parts of ethylene propylene diene rubber, 20 parts of neoprene, 10 parts of aramid fiber,
22 parts of carbon nano-fiber, 2 parts of stearic acid, 3 parts of zinc oxide, 4 parts of magnesia, 10 parts of silicones, 20 parts of phenolic resin, trapezoidal phenyl
30 parts of oligomeric silsesquioxane, eight ethenyl cage model oligomeric silsesquioxanes, 25 parts of mills are eventually adding peroxide to uniform mixing
Change 4 parts of diisopropylbenzene (DIPB), is kneaded, thin logical uniform, slice.Vulcanize at 160 DEG C of vulcanizing press 40 minutes and be molded, obtains the present invention
The polyhedral oligomeric silsesquioxane filling EPDM of the resistance to ablation heat insulation layers being related to.
The polyhedral oligomeric silsesquioxane filling EPDM of the resistance to ablation heat insulation layers of acquisition are as shown in Figure 1, its oxy-acetylene line is burnt
Erosion rate：0.025mm/s.
Comparative example
Sequentially added in 25 DEG C of two-roll mills 80 parts of ethylene propylene diene rubber, 20 parts of neoprene, 10 parts of aramid fiber,
22 parts of carbon nano-fiber, 2 parts of stearic acid, 3 parts of zinc oxide, 4 parts of magnesia, 10 parts of silicones, 20 parts of phenolic resin, trapezoidal phenyl
30 parts of mills of oligomeric silsesquioxane are eventually adding 4 parts of cumyl peroxide to uniform mixing, are kneaded, thin logical uniform, go out
Piece.Vulcanize at 160 DEG C of vulcanizing press 40 minutes and be molded, obtains polyhedral oligomeric silsesquioxane filling of the present invention
The EPDM of resistance to ablation heat insulation layers.Obtain contrast sample.
The polyhedral oligomeric silsesquioxane filling EPDM of the resistance to ablation heat insulation layers of acquisition are as shown in Fig. 2, its oxy-acetylene line is burnt
Erosion rate：0.078mm/s.
Product utilization POSS modifying agent of the present invention realizes that POSS exists it can be seen from above-described embodiment 1 and comparative example 1
Graft modification on EPDM rubber base material, while the excellent POSS of high temperature resistance, reinforcing agent, resin and organic fiber are added,
Significantly improve the ablation resistance of EPDM heat insulation layers.And compared to only with inertia polyhedral oligomeric silsesquioxane heat insulation layer,
Product ablation resistance of the present invention is greatly lowered, and carbon-coating is finer and close.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.Therefore, protection scope of the present invention is answered
This is subject to the protection scope in claims.
Claims (10)
1. a kind of polyhedral oligomeric silsesquioxane fills resistance to ablation EPDM rubber insulation, it is characterised in that：It is under
The component for stating mass parts is constituted：
2. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The Third monomer of the ethylene propylene diene rubber is ethylidene norbornene, and the ethylidene norbornene is in EPDM
Content in rubber is 5.0%-12.0%；And the ethylene contents in ethylene propylene diene rubber are 53.0%~59.0%.
3. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The neoprene is non-sulfur-modified neoprene.
4. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The reinforcing agent is one or more mixing in carbon nanotube, carbon nano-fiber, carbon black and white carbon.
5. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The organic fiber is Fanglun 1414, polysulphonamide fiber, the double oxazoles of polyparaphenylene's benzo
One or more mixing in fiber, polyacrylonitrile fibre.
6. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The fire resistant resin is one or more mixing in silicones, phenolic resin, polyimide resin.
7. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The high temperature resistant polyhedral oligomeric silsesquioxane is trapezoidal phenyl oligomeric silsesquioxane, octaphenyl cage modle is low
In polysilsesquioxane and phosphorous polyhedral oligomeric silsesquioxane and other high temperature resistant polyhedral oligomeric silsesquioxane compounds
One or more mixing.
8. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The modifying agent is mono-vinyl polyhedral oligomeric silsesquioxane, bi-vinyl polyhedral oligomeric silsesquioxane, four
Ethenyl cage model oligomeric silsesquioxane, eight ethenyl cage model oligomeric silsesquioxanes, phenyl vinyl polyhedral oligomeric sesquialter silicon
The polyhedral oligomeric silsesquioxane of oxygen alkane, isobutyl vinyl ether-glycidyl polyhedral oligomeric silsesquioxane and other carbon-carbon double bonds groups
In one or more mixing.
9. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The metal oxide is magnesia and/or zinc oxide.
10. polyhedral oligomeric silsesquioxane according to claim 1 fills resistance to ablation EPDM rubber insulation,
It is characterized in that：The vulcanizing agent is cumyl peroxide, 2,5- dimethyl -2,5- diperoxy benzene methyls hexane, two tertiary fourths
Base peroxide, 2,5- dimethyl -2,5- dual-tert-butyl peroxies hexane, 2,5- dimethyl -2,5- dual-tert-butyl peroxies -3-
Hexin, benzoyl peroxide, Isosorbide-5-Nitrae-dual-tert-butyl peroxy isopropyl base benzene, 1,1- dual-tert-butyl peroxides butylcyclohexane, 1,1-, bis- uncles
One or more mixing in butyl peroxy -3,3,5- trimethyl-cyclohexanes and other organic peroxide vulcanizing agents.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135073A (en) * | 2018-08-30 | 2019-01-04 | 北京理工大学 | A kind of resistance to ablation ternary ethlene propyene rubbercompound material and preparation method thereof |
| CN109251423A (en) * | 2018-09-13 | 2019-01-22 | 天津大学 | Trap based on POSS modified EPT rubber regulates and controls method |
| CN109294077A (en) * | 2018-09-13 | 2019-02-01 | 天津大学 | Electric branch suppressing method based on POSS regulation ethylene propylene diene rubber |
| CN109851924A (en) * | 2018-12-05 | 2019-06-07 | 湖北航天化学技术研究所 | A kind of EPDM insulation layer material and its preparation method and application |
| CN110041612A (en) * | 2019-04-01 | 2019-07-23 | 四川大学 | Oligomeric silsesquioxane increase-volume and synergistic halogen-free flame retardant polypropylene composite material and preparation method thereof |
| CN110359421A (en) * | 2019-07-30 | 2019-10-22 | 沈阳化大高分子材料研发中心有限公司 | A kind of long life high-voltage water blockoff rubber pneumatic bag and production technology |
| CN110591346A (en) * | 2019-09-17 | 2019-12-20 | 湖北洋田塑料制品有限公司 | High-temperature-resistant oil-modified nylon 6 composite material and preparation method thereof |
| CN111087680A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Low-VOC low-odor master batch for polypropylene, preparation method and application thereof, and method for reducing VOC content in polypropylene |
| CN111087679A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Low-VOC low-odor polypropylene resin composition and preparation method thereof |
| CN112175304A (en) * | 2020-10-20 | 2021-01-05 | 西北工业大学 | POSS (polyhedral oligomeric silsesquioxane) modified ethylene propylene diene monomer composite material with reaction type cage-type silsesquioxane structure and preparation method thereof |
| CN113292795A (en) * | 2021-06-18 | 2021-08-24 | 湖北航天化学技术研究所 | Rubber-combined low-ablation heat-insulating material and preparation method thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135073A (en) * | 2018-08-30 | 2019-01-04 | 北京理工大学 | A kind of resistance to ablation ternary ethlene propyene rubbercompound material and preparation method thereof |
| CN109251423A (en) * | 2018-09-13 | 2019-01-22 | 天津大学 | Trap based on POSS modified EPT rubber regulates and controls method |
| CN109294077A (en) * | 2018-09-13 | 2019-02-01 | 天津大学 | Electric branch suppressing method based on POSS regulation ethylene propylene diene rubber |
| CN111087680B (en) * | 2018-10-23 | 2021-12-31 | 中国石油化工股份有限公司 | Low-VOC low-odor master batch for polypropylene, preparation method and application thereof, and method for reducing VOC content in polypropylene |
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Application publication date: 20180810 |