CN107573601A - A kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling - Google Patents
A kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling Download PDFInfo
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Abstract
Provided by the present invention is a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling.Strengthen EPDM heat-insulating material poor flame retardant properties for current polyimide fiber, burning produces smog, polyimides PI fiber dispersions can meet to require, calendering process poor performance, the adhesive property of material and metal can not meet to require, maleic anhydride component not environmentally property the shortcomings that, the invention provides a kind of anti-yaw damper EPDM heat-insulating material formula of polyimide fiber filling and polyimide fiber pretreatment preparation technology and the rubber compounding technique of formula, formula constituent includes ethylene propylene diene rubber, CSM rubber, liquid rubber, zinc oxide, stearic acid, altax, diphenylguanidine, machine oil, silica, halogen-free flame retardants, polyimides PI fibers, resistance to Ablative resin, cumyl peroxide, sulphur, antiager RD.
Description
Technical field
The present invention relates to a kind of internal insulation material in solid rocket motor case thermal protection field.
Background technology
Solid rocket motor case thermal protection field, heat-insulating material matrix were once used as internal insulation matrix both at home and abroad
Material mainly has nitrile rubber system, EPDM EPDM rubber system and silicon rubber system etc..Due to ethylene propylene diene rubber
System relative density is most light, and EPDM EPDM heat-insulating materials start to obtain extensively should in solid propellant rocket internal insulation
With, trident series missile, MX guided missiles such as the U.S., some guided missile models of Japanese M-5 rockets and Russia, Italy
Solid propellant rocket etc..The internal insulation of U.S.'s SRMU solid propellant rockets is filled by two kinds of different content Kevlar fibers
EPDM EPDM be made.Xi Ao Ker Co., Ltd is Marshall Space Flight Center（MSFC）It has developed a kind of SiO of filling2
EPDM EPDM polymer, it is highly useful resistance to ablative insulative material, can substitute the polymerization of some not reproductions
Thing base ablation heat build-up material.U.S.'s Pegasus XL then uses winding-type EPDM EPDM heat insulation layers.In terms of moulding process,
The U.S. develops one kind continuous fiber dipping EPDM EPDM, and then Wrapping formed patented technology, simplifies technique, carries
High automaticity and Forming Quality.This is the new breakthrough in technology, has been successfully applied to guided missile solid-rocket hair
Motivation.In China, solid rocket motor case thermal protection internal insulation also uses EPDM EPDM thermal insulation layer materials.On
The beginning of the nineties end of the eighties in century, domestic scientific research institutions and colleges and universities have started three for different model solid propellant rocket
The research work of first the third EPDM of second heat insulation layers is simultaneously applied.
Widely used fiber reinforcement EPDM EPDM prepares resistance to ablative composite material both at home and abroad at present, and is successfully applied to
In the solid propellant rocket heat-insulating material of Multiple Type.But used by most fiber reinforcement EPDM EPDM heat-insulating materials
Fibrous material is glass fibre, carbon fiber, aramid fiber.The inorfils such as glass fibre, carbon fiber have good resistance to ablation
Characteristic, but it processes the shortcomings that broken, density is of a relatively high.1991, Davidson successfully have developed aramid fiber enhancing
EPDM in heat-insulating material.1996, aramid fiber short fibre enhancing EPDM systems were used for interior heat-insulating material by Guillot, relatively
Synthetic fibre fiber.Glass fiber reinforcement EPDM EPDM heat-insulating materials improve Burning corrosion resistance energy, and the density of material also reduces
.In the 1960s, du pont company has started the related research work of polyimides PI fibers.20 end of the centurys are Russian
The high-strength and high-modulus polyimides PI fibers that intensity reaches 2 times of Kevlar49 are more reported, its mechanical property can be with carbon fiber
T700 matches in excellence or beauty, and quality then alleviates 20% than carbon fiber.The shortcomings that due to EPDM heat-insulating material low poles, make it different with other
The interface cohesive force of phase material material such as fibre reinforced materials is weaker.In the selection of fibre reinforced materials, such as glass fibre, carbon
The inorfils such as fiber have good resistance to ablation characteristics, but it be present and process the shortcomings that broken and density is high.At present
Most study is aramid fiber, and it has the characteristics of high intensity, high-modulus and high temperature resistant and carbon forming rate are high, but aramid fiber
Easy entanglement, dispersing uniformity is poor in elastomeric material, and its mechanical property is relatively low.Polyimides PI fibers compared with aramid fiber,
Polyimides PI fibers have following technical advantage：（1）Carbon content is high；（2）Thermostabilization is higher；（3）Self-extinguishment is more preferable；（4）No
Easy entanglement, the above feature all illustrate to make using the polyimides PI fibers of high carbon content, high temperature resistant, high intensity and high-modulus
For the filler of resistance to ablation of EPDM internal insulations, with respect to heat-insulating material in aramid fiber EPDM, its mechanical property can be significantly improved
And ablation resistance.
2013《Aerospace material work》6th the 45-48 pages of phase《Influence of the fibre structure to EPDM composite properties》
With 2013《Industrial & Engineering Chemistry Research》The 1284-1290 pages of volume 52
《Surface-Modified Polyimide Fiber-Filled Ethylene-Propylenediene Monomer
Insulations for a Solid Rocket Motor: Processing, Morphology, and Properties》
Report the performance of the EPDM EPDM materials containing polyimides PI fibers.
2013《Composites Part A: Applied Science and Manufacturing》Volume 44
8-15 pages《Development of polyimide-nanosilica filled EPDM based light rocket
motor insulator compound: Influence of polyimide-nanosilica loading on
thermal, ablation, and mechanical properties》Report polyimides PI fiber EPDMs EPDM
Quality of materials part is formulated：100 parts of EPDM EPDM rubber, 2 parts of stearic acid, 3.0 parts of maleic anhydride, polyimides PI
Fiber 0-10 parts, nano silicon 0-10 parts, 1.0 parts of age resistor, 5.0 parts of zinc oxide, 1.5 parts of accelerant MBT, accelerator
1.5 parts of TMTD, 1.0 parts of sulphur.And discuss its mechanical performance, ageing properties and hot property.The formula materials solid-rocket is sent out
Problems be present in motivation products application：Poor flame retardant properties, smog is produced when meeting flame combustion；Polyimides PI fibers are three
Dispersive property can not still meet to require in first EPDM rubber of second third；Calendering process poor performance；The adhesive property of material and metal is not
It can meet to require；Maleic anhydride component is flammable, it is poisonous, have corrosivity, excitant.
The content of the invention
Provided by the present invention is a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling.
Add for glass fibre in current glass fibre and fibre reinforced EPDM EPDM heat-insulating materials and carbon fiber
The shortcomings that work is broken, density is of a relatively high, strengthen easy aramid fiber in EPDM EPDM heat-insulating materials for aramid fiber
The shortcomings that entanglement, for above-mentioned polyimides PI fiber reinforcements EPDM EPDM Flame Retardancies can it is poor, burning generation smog,
Polyimides PI fiber dispersions can meet that the adhesive property of requirement, calendering process poor performance, material and metal can not expire
Foot requires, maleic anhydride component not environmentally property the shortcomings that, a kind of anti-burning of polyimide fiber filling provided by the invention
EPDM heat-insulating material is lost, disclosure satisfy that Design of Solid Propellant Rocket Engine requirement and solid propellant rocket production will
Ask.
The technical solution adopted in the present invention:Rubber is EPDM EPDM rubber；Silica is reinforcing agent；Stearic acid
For plasticizer；Reinforcing fiber is polyimides PI fibers；Diphenylguanidine and altax are accelerator；Sulphur is vulcanizing agent；Using
Environment-friendly type antiager RD is antiager；Using low-smoke non-halogen flame-retardant agent as flame-retardant system, smog performance is reduced；Changed using resin
The viscosity of kind material；Using resin modified EPDM, the mechanical property of material is improved；Using liquid ethylene-propylene-diene rubber, promote
Enter fiber dispersing uniformity in the material and increase interfacial adhesion strength；Improve the processing performance of material using machine oil.This hair
Without maleic anhydride not environmentally, antioxidant D component in bright technical scheme.
Specifically mass parts basic components are：Ethylene propylene diene rubber, 100 parts；Liquid rubber, 4.0~6.0 parts；Zinc oxide,
5.0 part；Stearic acid, 1.0~2.0 parts；Altax, 3.0~6.0 parts；Diphenylguanidine, 0.5~2 part；Machine oil, 10 parts；Titanium dioxide
Silicon, 30 parts；Halogen-free flame retardants, 14.0~18.0 parts；Polyimides PI fibers, 3~7 parts；Resistance to Ablative resin, 10 parts；Sulphur,
0.5~1.5 part；Antiager RD, 1.0~2.0 parts.
Further to improve the performance of material heat-insulating material of the present invention, add cumyl peroxide, and sulphur for compounding sulphur
Change system, promote curability, reduce curing temperature；The ageing-resistant performance of material, fire resistance and resistance to are improved using CSM rubber
Oiliness energy performance.
Specific mass parts improve formula：Ethylene propylene diene rubber, 100 parts；CSM rubber, 4.0~6.0 parts；Liquid rubber
Glue, 4.0~6.0 parts；Zinc oxide, 5.0 parts；Stearic acid, 1.0~2.0 parts；Altax, 3.0~6.0 parts；Diphenylguanidine, 0.5
~2 parts；Machine oil, 10 parts；Silica, 30 parts；Halogen-free flame retardants, 14.0~18.0 parts；Polyimides PI fibers, 3~7 parts；
Resistance to Ablative resin, 10 parts；Cumyl peroxide, 1.5~2.5 parts；Sulphur, 0.5~1.5 part；Antiager RD, 1.0~2.0
Part.
A kind of technology of preparing of the anti-yaw damper EPDM heat-insulating material of polyimide fiber filling provided by the present invention
For two links, first, fiber pre-processes, second, rubber compounding.The purpose of fiber pretreatment is by controlling reamer rotating speed, twisting
The broken time obtains varigrained particle, and agitated mixed zone animal material disperses to move upwards along pot wall, and cutting reamer is quick
Fiber surface is divided into the surface area of " groove " increase fiber, and improves fiber surface activity.Rubber compounding is added in component
Afterwards, control melting temperature exists（40~50）Thin logical, slice after DEG C being kneaded uniformly, is prepared into solid rocket motor case thermal protection
Heat-insulating material.
1) polyimides PI fibers pretreatment preparation technology is as follows：
A) fiber wash, (10~15) %PI fibers, (85~90) % cleaning solvent ethanol are put into the work of fiber wash device
Interior, pass through（40~50）DEG C heating, stirring, the fiber that washing is completed is taken out after (0.5~1) h;
B) solvent removal, the fiber for washing completion is poured into centrifuge desolvation (1~3) min, room temperature is dried;
C) fiber surface is pre-processed, and the polyimides PI fibers that room temperature is dried are poured into the operating room of Fiber strength machine
It is interior, mixed by adjusting in double-speed motor control operating room's pot, cutting reamer rotating speed exists（30~60）R/min, and pass through
Peristaltic pump to work household sprays（5~30）%KH-550/ ethanol surface pretreatment agents, operation（30~40）Discharged after s;
D) fiber disperses：Using fiber decentralized processing equipment, controlled by adjustable mechanical power dispersal device and give fiber roller rotating speed ＜
2r/min, spiny hair roller rotating speed ＜ 900r/min.
2）The rubber compounding technique of basic components：
By recipe calculation amount, ethylene propylene diene rubber, liquid rubber are put into open or internal rubber mixer and plasticated, then according to
Secondary input zinc oxide, stearic acid part, altax and diphenylguanidine, machine oil, silica, halogen-free flame retardants, polyimides PI
Fiber, resistance to Ablative resin, antiager RD, sulphur, control melting temperature exist（40~50）Thin logical, slice after DEG C being kneaded uniformly, system
The standby anti-yaw damper EPDM heat-insulating material into polyimide fiber filling.
3）Improve the rubber compounding technique of formula：
By recipe calculation amount, ethylene propylene diene rubber, CSM rubber, liquid rubber are put into open or internal rubber mixer
Plasticate, then put into zinc oxide, stearic acid, altax, diphenylguanidine, machine oil, silica, halogen-free flame retardants, polyamides Asia successively
Amine PI fibers, resistance to Ablative resin, antiager RD, cumyl peroxide, sulphur, control melting temperature exist（40~50）DEG C be kneaded
Thin logical, slice after uniformly, it is prepared into the anti-yaw damper EPDM heat-insulating material of polyimide fiber filling.
Embodiment
The present invention according to aforementioned base formula, improve formula, polyimides PI fibers pre-process preparation technology and with
Rubber compounding technique corresponding to side has carried out trial-production production, and concrete outcome is as follows.
Specific implementation 1：Ethylene propylene diene rubber, 100 parts；CSM rubber, 5.5 parts；Liquid rubber, 5.5 parts；Zinc oxide,
5.0 part；Stearic acid, 1.5 parts；Altax, 4.5 parts；Diphenylguanidine, 1 part；Machine oil, 10 parts；Silica, 30 parts；Halogen hinders
Combustion agent, 15 parts；Polyimides PI fibers, 5 parts；Resistance to Ablative resin, 10 parts；Cumyl peroxide, 2 parts；Sulphur, 1 part；It is anti-ageing
Agent RD, heat-insulating material prepared by 1 part of recipe ingredient mixing, its tensile strength 7.61Mpa, elongation 713%, the g of density 1.08/
Cm3, oxy-acetylene linear ablative rate 0.08mm/s, and the curability of material is excellent, and ablation resistance is excellent, calendering process performance
It is excellent.
Specific implementation 2：Ethylene propylene diene rubber, 100 parts；CSM rubber, 4.0 parts；Liquid rubber, 4.0 parts；Zinc oxide,
5.0 part；Stearic acid, 1.0 parts；Altax, 3.0 parts；Diphenylguanidine, 0.5 part；Machine oil, 10 parts；Silica, 30 parts；Halogen
Fire retardant, 14.0 parts；Polyimides PI fibers, 3 parts；Resistance to Ablative resin, 10 parts；Cumyl peroxide, 1.5 parts；Sulphur,
0.5 part；Antiager RD, 1.0 parts of recipe ingredients are kneaded the heat-insulating material prepared, its tensile strength 7.92Mpa, elongation 689%,
1.06 g of density/cm3, oxy-acetylene linear ablative rate 0.10mm/s, and the curability of material is excellent, ablation resistance is excellent,
Calendering process function admirable.
Specific implementation 3：Ethylene propylene diene rubber, 100 parts；CSM rubber, 6.0 parts；Liquid rubber, 6.0 parts；Zinc oxide,
5.0 part；Stearic acid, 2.0 parts；Altax, 6.0 parts；Diphenylguanidine, 2 parts；Machine oil, 10 parts；Silica, 30 parts；Halogen hinders
Combustion agent, 18.0 parts；Polyimides PI fibers, 7 parts；Resistance to Ablative resin, 10 parts；Cumyl peroxide, 2.5 parts；Sulphur, 1.5
Part；Antiager RD, 2.0 parts of recipe ingredients are kneaded the heat-insulating material prepared, its tensile strength 7.09Mpa, elongation 762%, density
1.09 g/cm3, oxy-acetylene linear ablative rate 0.08mm/s, and the curability of material is excellent, and ablation resistance is excellent, is kneaded
Processing performance is excellent.
Specific implementation 4：Ethylene propylene diene rubber, 100 parts；Liquid rubber, 5.0 parts；Zinc oxide, 5.0 parts；Stearic acid, 1.5
Part；Altax, 4.0 parts；Diphenylguanidine, 1 part；Machine oil, 10 parts；Silica, 30 parts；Halogen-free flame retardants, 15.0 parts；Polyamides
Imines PI fibers, 5 parts；Resistance to Ablative resin, 10 parts；Sulphur, 1 part；Antiager RD, 1.0 parts of recipe ingredients are kneaded the exhausted of preparation
Hot material, its tensile strength 6.80Mpa, elongation 642%, 1.09 g of density/cm3, oxy-acetylene linear ablative rate 0.11mm/s, and
And the curability of material meets to require, ablation resistance meets that requirement, calendering process performance meet to require.
Specific implementation 5：Ethylene propylene diene rubber, 100 parts；Liquid rubber, 4.0；Zinc oxide, 5.0 parts；Stearic acid, 1.0 parts；
Altax, 3.0 parts；Diphenylguanidine, 0.5 part；Machine oil, 10 parts；Silica, 30 parts；Halogen-free flame retardants, 14.0 parts；Polyamides is sub-
Amine PI fibers, 3 parts；Resistance to Ablative resin, 10 parts；Sulphur, 1.5 parts；Antiager RD, 1.0 parts of recipe ingredients are kneaded the exhausted of preparation
Hot material, its tensile strength 5.81Mpa, elongation 603%, 1.06 g of density/cm3, oxy-acetylene linear ablative rate 0.12mm/s, and
And the curability of material meets to require, ablation resistance meets that requirement, calendering process performance meet to require.
Specific implementation 6：Ethylene propylene diene rubber, 100 parts；Liquid rubber, 6.0 parts；Zinc oxide, 5.0 parts；Stearic acid,
2.0 part；Altax, 6.0 parts；Diphenylguanidine, 2 parts；Machine oil, 10 parts；Silica, 30 parts；Halogen-free flame retardants, 18.0
Part；Polyimides PI fibers, 7 parts；Resistance to Ablative resin, 10 parts；Sulphur, 1.5 parts；Antiager RD, 2.0 parts of recipe ingredients mix
Standby heat-insulating material is refined, its tensile strength 6.26Mpa, elongation 653%, 1.08 g of density/cm3, oxy-acetylene linear ablative rate
0.10mm/s, and the curability of material meets to require, and ablation resistance meets that requirement, calendering process performance meet to require.
Claims (7)
1. a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling, including solid ethylene propylene diene rubber, fiber
Material, fire proofing, reinforcing agent, plasticizer, vulcanizing agent, antiager, accelerator, activating agent, process auxiliaries, it is characterised in that
Fibrous material is polyimides PI fibers, fire proofing is halogen-free flame retardants, reinforcing agent is silica, plasticizer is stearic
Acid, vulcanizing agent are sulphur, antiager is antiager RD, and activating agent is zinc oxide, accelerator is diphenylguanidine and altax, work
Skill auxiliary agent is machine oil, then adds liquid ethylene-propylene-diene rubber and the resin of resistance to burning.
2. a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling according to claim 1, its feature
It is, in addition to vulcanizing agent cumyl peroxide, CSM rubber.
3. a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling according to claim 1, its feature
Be, by quality be 100 parts of ethylene propylene diene rubbers based on mass parts formula be：100 parts of ethylene propylene diene rubber, liquid rubber
4.0~6.0 parts, 5.0 parts of zinc oxide, 1.0~2.0 parts of stearic acid, 3.0~6.0 parts of altax, 0.5~2 part of diphenylguanidine,
10 parts of machine oil, 30 parts of silica, 14.0~18.0 parts of halogen-free flame retardants, 3~7 parts of polyimide fiber PI fibers, resistance to ablation
10 parts of resin, 0.5~1.5 part of sulphur, 1.0~2.0 parts of antiager RD.
4. a kind of anti-yaw damper EPDM heat-insulating material of polyimide fiber filling according to claim 2, its feature
Be, by quality be 100 parts of ethylene propylene diene rubbers based on mass parts formula be：100 parts of ethylene propylene diene rubber, CSM rubber
4.0~6.0 parts, 4.0~6.0 parts of liquid rubber, 5.0 parts of zinc oxide, 1.0~2.0 parts of stearic acid, altax 3.0~6.0
Part, 0.5~2 part of diphenylguanidine, 10 parts of machine oil, 30 parts of silica, 14.0~18.0 parts of halogen-free flame retardants, polyimides fibre
Tie up 3~7 parts of PI fibers, resistance to 10 parts of Ablative resin, 1.5~2.5 parts of cumyl peroxide, 0.5~1.5 part of sulphur, antiager
1.0~2.0 parts of RD.
5. a kind of anti-yaw damper EPDM of any polyimide fiber filling prepared as described in claim 1 or 3 is adiabatic
Material, it is characterised in that rubber compounding manages step and is：By recipe calculation amount, ethylene propylene diene rubber, liquid rubber are put into out
Put in formula or internal rubber mixer and plasticate, then put into zinc oxide, stearic acid part, altax and diphenylguanidine, machine oil, two successively
Silica, halogen-free flame retardants, polyimide fiber PI fibers, resistance to Ablative resin, antiager RD, sulphur, control melting temperature exist
（40~50）Thin logical, slice after DEG C being kneaded uniformly, it is prepared into the anti-yaw damper EPDM heat-insulating material of polyimide fiber filling.
6. a kind of anti-yaw damper EPDM heat-insulating material of the polyimide fiber filling prepared as described in claim 2 or 4, its
It is characterised by that rubber compounding processing step is：By recipe calculation amount, ethylene propylene diene rubber, CSM rubber, liquid rubber are put into
Plasticated in open or internal rubber mixer, then put into zinc oxide, stearic acid, altax 3, diphenylguanidine, machine oil, two successively
Silica, halogen-free flame retardants, polyimide fiber PI fibers, resistance to Ablative resin, antiager RD, cumyl peroxide, sulphur,
Control melting temperature exists（40~50）Thin logical, slice after DEG C being kneaded uniformly, it is prepared into the anti-yaw damper three of polyimide fiber filling
First heat-insulating material of second third.
A kind of 7. anti-yaw damper EPDM of any polyimide fiber filling prepared as described in claim 1,2,3 or 4
Heat-insulating material, it is characterised in that including polyimide fiber PI fiber pre-treatment steps：
A) fiber wash, (10~15) %PI fibers, (85~90) % cleaning solvent ethanol are put into the work of fiber wash device
Interior, pass through（40~50）DEG C heating, stirring, the fiber that washing is completed is taken out after (0.5~1) h;
B) solvent removal, the fiber for washing completion is poured into centrifuge desolvation (1~3) min, room temperature is dried;
C) fiber surface is pre-processed, and the polyimide fiber PI fibers that room temperature is dried are poured into the work of Fiber strength machine
Interior, mixed by adjusting in double-speed motor control operating room's pot, cutting reamer rotating speed exists（30~60）R/min, and lead to
Peristaltic pump is crossed to work household sprays（5~30）%KH-550/ ethanol surface pretreatment agents, operation（30~40）Discharged after s;
D) fiber disperses：Using fiber decentralized processing equipment, controlled by adjustable mechanical power dispersal device and give fiber roller rotating speed ＜
2r/min, spiny hair roller rotating speed ＜ 900r/min.
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Cited By (4)
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| CN109593359A (en) * | 2018-12-07 | 2019-04-09 | 江苏先诺新材料科技有限公司 | A kind of preparation method of high filled polyimide pulp rubber master batch |
| CN109762215A (en) * | 2019-01-17 | 2019-05-17 | 北京化工大学 | High-performance polyimide long fiber reinforcement rubber composite material and preparation method thereof |
| CN112225998A (en) * | 2020-09-03 | 2021-01-15 | 湖北航天化学技术研究所 | Ablation-resistant heat-insulating material with excellent mechanical property for high-energy propellant and preparation method thereof |
| CN112724542A (en) * | 2021-01-14 | 2021-04-30 | 浙江大器高分子材料有限公司 | Magnetic rubber material and preparation method thereof |
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| CN109762215A (en) * | 2019-01-17 | 2019-05-17 | 北京化工大学 | High-performance polyimide long fiber reinforcement rubber composite material and preparation method thereof |
| CN112225998A (en) * | 2020-09-03 | 2021-01-15 | 湖北航天化学技术研究所 | Ablation-resistant heat-insulating material with excellent mechanical property for high-energy propellant and preparation method thereof |
| CN112225998B (en) * | 2020-09-03 | 2023-03-10 | 湖北航天化学技术研究所 | Ablation-resistant thermal insulation material with excellent mechanical property for high-energy propellant and preparation method thereof |
| CN112724542A (en) * | 2021-01-14 | 2021-04-30 | 浙江大器高分子材料有限公司 | Magnetic rubber material and preparation method thereof |
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Application publication date: 20180112 |