CN105585848B - Solid propellant rocket liner molding silicone rubber air capsule material and preparation method thereof - Google Patents
Solid propellant rocket liner molding silicone rubber air capsule material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to one kind in the case where EPDM heat-insulating material forms complex working condition environment, the long-life high temperature sulphurated siliastic material of the anti-degradation of high temperature resistant, is exclusively used in preparing solid space rocket engine liner molding auxiliary balloon.Its recipe ingredient (weight) is 100 parts of silicone rubber compounds, 30 ~ 50 parts of gas-phase silica, 5 ~ 10 parts of ageing-resistant additive A, 1 ~ 3 part of ageing-resistant additive B, 5 ~ 10 parts of ageing-resistant addition of C, 5 ~ 10 parts of silazane, 1 ~ 3 part of vulcanizing agent, it is mixing with the process that the silicon rubber prepares balloon mold, back mixing, molding, one step cure, bonding, post vulcanization, with the silicon rubber in sealing state, 150 DEG C of temperature, pressure 0.5MPa, in the presence of EPDM rubber insulation composite material, it used and does not fail through 200 hours, it can be applied to the liner molding auxiliary balloon material of the various pressure vessel such as solid space rocket engine.
Description
Technical field
The invention belongs to solid space rocket engine technical field, in particular to a kind of solid propellant rocket liner at
Type such as solid propellant rocket internal insulation molding silicon rubber composite material and preparation method thereof.
Background technique
The molding of Solid Rocket Motors For Aerospace liner generallys use a kind of silicone rubber air sacs assistant formation technique, main
Principle is pressed by the regulation of internal pressure to composite body, and be allowed to using air bag as core model when composite molding
Curing molding.Silicon rubber inflatable bag core mold is flexible to be compared with compression molding, it is easy to accomplish complex structural member it is integrally formed,
It fills, demould simple and efficient, a large amount of working hours can be saved, simplify moulding process flow process, opposite conventional metals and other polymers core model,
With apparent cost advantage.
Dedicated silastic material for air bag assistant formation technique requires have higher thermal stability and synthesis ageing-resistant
Performance, under heat and pressure resistance to rotten or resistance to softening, dimensionally stable, high stretch modulus, high-tear strength, Gao Duan after reuse
Split elongation etc..For example, being applied to the molding Silicon rubber inflatable bag of solid propellant rocket liner, due to being chronically at temperature
150 DEG C, in the enclosed environment of 0.1 ~ 0.7MPa of internal pressure, the inner lining material that be resistant to complicated composition (comprising rubber, all kinds of inorganic is filled out
Material, expanding material, auxiliary agent, fire retardant, catalyst, crosslinking agent etc.) physics repeatedly and chemical action, chemically-resistant heat-resisting to material
The comprehensive ageing-resistant performance such as effect, resistance to peroxide, pressure resistance proposes very high requirement.Current commercialized Related product, is adopted
It is made with 110-2 glue of the material of matrix, addition white carbon black, fillers and the additive such as three oxygen, two iron, in the present context small through 6
Shi Laohua, discovery silicon rubber is seriously tacky after solution is created, and degradation reaction has occurred.
In addition, in the prior art, there are many high temperature resistant, not aging, non-degradable sulphurated siliastic.Such as in Chinese patent
" anti-degradation room temperature vulcanized silicone rubber ", Authorization Notice No. are that CN1410487A is disclosed under a kind of sealing state through 24 hours 150
DEG C high temperature, not aging, non-degradable casting glue, but not yet discovery meets similar this kind of solid-rocket of solid propellant rocket and starts
Machine liner forms work condition environment, and (sealing state, 150 DEG C of temperature, 0.1 ~ 0.7MPa of pressure, EPDM are insulated layer material and its divide
Solution product) and be able to use 200 hours long-life sulphurated siliastic material technology.In addition, by polytetrafluoroethylene (PTFE), carbon modified
The ageing-resistant additive that nanotube, chitosan and transition metal oxide collaboration are used as silastic material is also not reported so far.
Summary of the invention
In view of the deficiencies of the prior art, the present invention solves the problems, such as to be to provide a kind of solid propellant rocket liner molding silicon
The formula and preparation method thereof of rubber pneumatic bag material, substantially to extend silicone rubber air capsule material under closed complex working condition environment
Service life improves the molding reliability of solid propellant rocket liner.Silicon rubber inflatable bag mold materials provided by the present invention
Liner suitable for solid propellant rocket forms.
Silicone rubber air capsule material of the invention can be fixed on solid propellant rocket inner lining surface by certain air pressure, rise
To the support molding effect of liner, to guarantee the integrality of liner and the reliability of work.The solid propellant rocket liner at
Type silicone rubber air capsule material includes following components according to the weight ratio:
(1) silicone rubber compounds 100-120 parts；
(2) ageing-resistant additive A 5-10 parts；
(3) 1 ~ 3 part of ageing-resistant additive B；
(4) 5 ~ 10 parts of ageing-resistant addition of C；
(5) reinforced filling 30-50 parts；
(6) vulcanizing agent 0.5-3 parts；
(7) 5 ~ 12 parts of antistructurizing agent；
(8) 1 ~ 5 part of coupling agent.
(9) 5 ~ 10 parts of process auxiliaries.
Further, the silicone rubber compounds are one or both of methyl vinyl silicone rubber, phenyl siloxane rubber.
Further, the ageing-resistant additive A is the single or composite oxides of manganese, iron, cerium.
It is a further object to provide a kind of preparation methods of above-mentioned silicone rubber air capsule material, use silicone rubber air
The technical process of capsule material are as follows:
Firstly, at room temperature, successively by weight ratio by matrix resin, reinforced filling, resistance to Peroxide Additives
It is put into progress room temperature mixing in open mill.
Roll spacing is adjusted to 2mm after breaking gel；Silane coupling agent, constitution controller are slowly added to after packet roller；Sulphur is added after mixing
Agent, bottom sheet after mixing.
Then, sizing material is pressed by certain thickness blob of viscose by screw extruder and press according to model demand, by glue
Block slice (thickness 2mm) on two roller machine；
Production mold finally is required according to container model, by above-mentioned silicon rubber raw cook packet on mold, passes through shaping, calendering
The processes such as overlap edge are that balloon size meets drawing requirement, then carry out one step cure under normal pressure, and heat transfer medium is hot-air,
160 ~ 170 DEG C of curing temperature, vulcanization time 30min；Check the air-tightness of air bag, it is qualified then carry out post vulcanization.
The invention has the following advantages:
(1) silicone rubber air capsule material of the invention replaces existing product, makes the molding air bag of solid propellant rocket liner
Service life extends to 200 hours, the air bag cost of molding process by every 100 times 100,000 yuan be reduced to 10,000 5 thousand yuan hereinafter, and
And the vulcanized rubber is easy to use, is easy to keep, raw material are easy to obtain.
(2) the silicone rubber air capsule material is used, high-temperature silicon disulfide rubber can be placed, high temperature drop occurs in sealed states
Solution reaction, solves hidden danger of quality, prevents scrap of the product, largely improve reliability and the service life of product.
Specific embodiment
The technical scheme of the present invention will be further described with reference to embodiments.
Solid propellant rocket liner molding silicone rubber air capsule material of the invention, includes with the following group according to the weight ratio
Point:
(1) silicone rubber compounds 100-120 parts；
(2) ageing-resistant additive A 5-10 parts；
(3) 1 ~ 3 part of ageing-resistant additive B；
(4) 5 ~ 10 parts of ageing-resistant addition of C；
(5) reinforced filling 30-50 parts；
(6) vulcanizing agent 0.5-3 parts；
(7) 5 ~ 12 parts of antistructurizing agent；
(8) 1 ~ 5 part of coupling agent.
(9) 5 ~ 10 parts of process auxiliaries.
Further, the silicone rubber compounds are methyl vinyl silicone rubber, phenyl siloxane rubber (including three kinds basic, normal, high)
One or both of, it is the matrix sizing material of Silicon rubber inflatable bag mold materials.Raw rubber can be increased using the silicon rubber of unique construction
The steric hindrance of main chain prevents silicon rubber backbone rearrangement from degrading, to increase substantially the heat resistance of silicon rubber composite material.
Preferably, the ageing-resistant additive A is transition metal mixed oxides.Such compound can be by preventing freely
The chain growth of base reduces attack of the active oxygen to silicon rubber side group, thus the thermal decomposition aging of substantially reduced silicon rubber.Pass through system
The compound of this standby a few class compound can effectively play them to synergistic effect ageing-resistant under complex working condition environment.It is made
Standby technique is as follows: at room temperature, preparing two kinds or several of nickel, cobalt, copper, tin, manganese, iron, cerium, lanthanum etc. using sol-gal process
Gel is placed in 110 DEG C of drying overnight by composite oxides gel, and 400 DEG C of pre-burnings 1h, 800 DEG C of calcining 2h are obtained compound after cooling
Oxide samples save at 0 ~ 30 DEG C of hermetically drying.
Further, the ageing-resistant additive B is that hydroxyl or amino modified multi-wall carbon nano-tube tube material or low molecule shell are poly-
One or both of sugar.Carbon nano-tube material more difficult dispersion in silicon rubber, it is therefore desirable to first use following pre-dispersed work
Skill is handled: carbon nanotube being added in appropriate dimethylbenzene, ultrasonic disperse 1 hour or so.It will a small amount of more ethylene liquids
Silicon rubber is added in xylene solution, after dissolution is sufficiently stirred, withs a small amount of multiple mode while being stirred ultrasound
The xylene solution of above-mentioned carbon nanotube is added, continues ultrasound 30min after the completion of being added.Then dimethylbenzene is sloughed rapidly, is sealed
It is good spare.The chitosan of low molecular weight is better than the chitosan of high molecular weight in terms of understanding superoxide anion and hydroxyl radical free radical,
It can directly add or modified carbon nano-tube collaboration is cooperated to use in silicon rubber.
Further, the ageing-resistant addition of C be one of ptfe emulsion or superfine powder of polytetrafluoroethylene or
Two kinds.This kind of material has very high dispersibility, can be with other materials homogeneous blend.Resistance to strong acid, highly basic, strong oxidizer.
Further, the reinforced filling is gas-phase silica, high-intensitive white carbon black, acetylene carbon black, diatomite, montmorillonite etc.
Filler, wherein the trade mark of white carbon black includes that M5, Ts720, S-600, HB-612 or HB-620, Nano carbon white and Ji are invincible
One of silanization white carbon black is several.White carbon black is considered as that raw-silastic continuously molecule is easier to the reinforcing effect of silicon rubber
It is adsorbed on the Si0 of dispersion2Particle surface makes interparticle distance from particle not holding any government official post diameter is less than, and the part chain link of raw rubber molecule is sequentially
Arrangement, to generate crystallization effect, enhances intermolecular attraction in adsorption layer；In addition, the Si-O key in raw rubber molecule
Or its terminal hydroxy group can be with Si02The Si-OH base on surface forms physics or chemical bonding, improves the physical and mechanical property of vulcanizate.
Variety classes, the filler of different-grain diameter are very big to the reinforcing effect difference of silicon rubber.
Further, the vulcanizing agent is benzoyl peroxide, cumyl peroxide, 2,4- dichlorobenzoperoxide
(DCEP), t-butyl perbenzoate, peroxidating di tert butyl carbonate, in the 2,5-tert-butyl peroxy of dimethyl-2,5-two bases-hexane
One or two, the raw-silastic continuously of high viscid plasticity state can be made to be changed into the elastic state silicon rubber material of tridimensional network
Material.
Further, the antistructurizing agent is hexamethyl cyclotrisilazane, octamethylcyclotetrasilazane, two silicon of diphenyl
One or both of alcohol, hydroxy silicon oil, the inorganic agent as reinforced filling surface texture use, and can effectively adjust filler table
Hydroxy radical content between face inhibits Si-OH too high levels under high temperature that silicon rubber thermal rearrangement is caused to be degraded.
Further, the coupling agent is epoxy coupling agents and acryloxy coupling agent, epoxy coupling agents and acryloyl-oxy
Base coupling agent be southern big -42 silane coupling agents, A-151 silane coupling agent, γ-glycidol ether propyl trimethoxy silicane and
One or both of γ-methacryloxypropyl trimethoxy silane is bonded using epoxy, acryloxy coupling agent
Stable chemical covalent bonds can be formed, bonding persistence and stability between filler and matrix resin are greatly improved, to change
Kind processing performance, improves ageing-resistant performance.
Solid propellant rocket liner molding silicone rubber air capsule material of the invention may also include process auxiliaries, ternary second
Third insulation layer material.
Process auxiliaries refer to stearic acid, zinc stearate, zinc oxide, dioctyl sebacate, dibutyl phthalate, lemon
One of triethylenetetraminehexaacetic acid ester, chlorinated paraffin -42, tricresyl phosphate, tributyl 2-acetylcitrate are several, are kneaded for improving
The processing performance of glue prevents roll banding and the phenomenon that can not forming occurs.
It is matrix that EPDM insulation layer material, which is by ethylene propylene diene rubber, is proportionally added into fire retardant, carbon fiber or virtue
A kind of elastomer composite that synthetic fibre fiber, white carbon black, curing agent and other auxiliary agent room temperatures are kneaded and are vulcanized under normal pressure
Material is one of current most common solid propellant rocket internal insulation material.
Under coupling agent, vulcanizing agent effect open loop, hydrolysis, condensation, esterification occur for silicone rubber matrix.
Please refer to the of the invention 5 Silicon rubber inflatable bag material prescription enumerated in table 1.
The solid propellant rocket liner molding silicone rubber air capsule material of the invention of table 1 and comparative example proportion are (single
Position: %)
| Material name | Formula 1 | Formula 2 | Formula 3 | Formula 4 | Formula 5 | Comparative example |
| Phenyl siloxane rubber resin | 100 | 100 | 100 | 100 | 100 | 0 |
| Methyl vinyl silicone rubber | / | / | / | / | / | 100 |
| Hydrophobic silicic aerogels | 30 | 40 | 25 | 40 | 35 | / |
| Fume colloidal silica | 20 | 10 | 25 | / | 15 | 40 |
| Metal composite oxide | 10 | 5 | 8 | 6 | 3 | 10 |
| Amino modified carbon nanotube | 1 | / | 0.5 | / | 0.8 | / |
| Hydroxyl modification carbon nanotube | / | 1 | 0.5 | / | 1 | / |
| Low molecular chitosan | / | 1 | 1 | 2 | 1.5 | / |
| Ptfe emulsion | 5 | 5 | 8 | 10 | 4 | / |
| Dioctyl sebacate | / | / | 3 | / | 1.5 | 2.5 |
| Zinc oxide | / | 5 | / | 5 | / | / |
| Stearic acid | 5 | / | / | / | / | |
| Zinc stearate | / | / | / | / | 5 | 5 |
| Silane coupling agent | 2.5 | 2.5 | 3 | 5 | 5 | 2.5 |
| Silazane | 3 | 3 | 5 | 5 | 5 | 3 |
| Vulcanizing agent | 3 | 3 | 3 | 3 | 3 | 3 |
Embodiment 1
High-temperature sulfuration silicon rubber raw rubber is machined in open type dual-roller cylinder refining glue at room temperature.It is pressed in table 1 first and is formulated 1 for first
Base phenyl siloxane rubber resin raw rubber is added on roller, after sizing material packet roller of machining, is gradually added filler (white carbon black, resistance to peroxide
Compound additive, coupling agent etc.).After sizing material thin logical 8 ~ 10 times after being kneaded uniformly, clot bottom sheet obtains rubber compound and deposits in drying
It is spare in device.Rubber compound carries out back mixing after placing 24 hours, carries out on open type dual-roller cylinder rubber mixing machine, when sizing material limbers up,
Surface is smooth, Bao Tong 5 ~ 10 times, can blanking slice.Then by silicon rubber gross rubber on open type dual-roller cylinder rubber mixing machine
Packet roller, is added crosslinking agent, catalyst etc., Bao Tong 10 times or so, by blob of viscose on two roller machine slice (thickness 2mm).Pressing force is held
Type number requires to prepare the mold (head, tail portion, shell portion are fabricated separately) for making capsule, then by silicon rubber raw cook packet in glue
On capsule mold, by processes such as shaping, calendering overlap edges, capsule size is made to meet the requirements, and in silicon rubber top covering cloth, fixed
Raw-silastic continuously capsule carries out one step cure under normal pressure, and heat transfer medium is hot-air, and curing temperature is 160 ~ 170 DEG C, vulcanization
Time about 30min.Finally by the capsule of different piece by adhesive be bonded together carry out post vulcanization (150 DEG C of condition ×
120min).
By the air bag made 150 DEG C of temperature, 0.1 ~ 0.7MPa of internal pressure enclosed environment under, based on material use item
Part carries out the artificial accelerated aging under molding simulation experimental condition in combination with standard GB/T/T 7141-1992, small through 200
When test process, air bag appearance is unchanged, after dissection sampling carry out Mechanics Performance Testing.Silicon rubber in practical application is simulated to be pressurized
It can be obtained by way of processing dress, the size of pressing force is indicated by the dependent variable of Control Assay.With firmness change 15
Degree and elongation rate of tensile failure change -50% and are used as rubber failure criteria, the results showed that 1 formula materials of case study on implementation can meet completely
The requirement to work 200 hours under conditions of 150 DEG C, 0.1 ~ 0.7MPa of internal pressure.
Embodiment 2
Prepare solid propellant rocket liner assistant formation Silicon rubber inflatable bag 2 by formula 2 in table 1, preparation method with
Embodiment 1 is identical.Gained bag material performance of the invention is shown in Table 2 embodiment 2.
Embodiment 3
Prepare solid propellant rocket liner assistant formation Silicon rubber inflatable bag 3 by formula 3 in table 1, preparation method with
Embodiment 1 is identical.Gained bag material performance of the invention is shown in Table 2 embodiment 3.
Embodiment 4
Prepare solid propellant rocket liner assistant formation Silicon rubber inflatable bag 4 by formula 4 in table 1, preparation method with
Embodiment 1 is identical.Gained bag material performance of the invention is shown in Table 2 embodiment 4.
Embodiment 5
Prepare solid propellant rocket liner assistant formation Silicon rubber inflatable bag 5 by formula 5 in table 1, preparation method with
Embodiment 1 is identical.Gained bag material performance of the invention is shown in Table 2 embodiment 5.
Comparative example
Silicone rubber air capsule material is prepared by the formula of comparative example in table 1, preparation method is same as Example 1, gained sheet
The performance of invention bag material is shown in Table 2 comparative example.
Mechanical property before and after the Silicon rubber inflatable bag material aging of the invention of table 2 and the compared with current material
* ageing time is 200 hours.
(according to GB/T528-1998 " measurement of vulcanized rubber or thermoplastic elastomer tensile stress-strain performance ", GB/
T529-1999 " measurement of vulcanized rubber or thermoplastic elastomer tearing strength ", GB/T15254-94 " vulcanized rubber and metal adhesive
180 ° of peel tests " in require cut into required shape.
Claims (5)
1. a kind of solid propellant rocket liner molding silicone rubber air capsule material, which is characterized in that the silicone rubber component packet
It includes by weight are as follows:
Silicone rubber compounds, 100 parts；
Ageing-resistant additive A, 5-10 parts；
Ageing-resistant additive B, 1 ~ 3 part；
Ageing-resistant addition of C, 5 ~ 10 parts
Reinforced filling, 30-50 parts；
Vulcanizing agent, 0.5-3 parts；
Antistructurizing agent, 5 ~ 12 parts；
Coupling agent, 1 ~ 5 part；
The ageing-resistant additive B is hydroxyl, amino or carboxy-modified carbon nano-tube material, low-molecular weight chitoglycan and its derivative
Object is therein any one or more of；
The silicone rubber compounds are one or both of methyl vinyl silicone rubber, phenyl siloxane rubber；
The ageing-resistant additive A is the single or composite oxides of manganese, iron, cerium；
The reinforced filling be fume colloidal silica Ts720, M5, HB-612 or HB-620, silanization white carbon black it is single or mixed
Close object；The ageing-resistant addition of C is the single or mixture of ptfe emulsion, superfine powder of polytetrafluoroethylene.
2. a kind of method for preparing solid propellant rocket liner molding silicone rubber air capsule material described in claim 1,
It is characterized in that, comprises the following steps that:
High-temperature sulfuration silicon rubber raw rubber is machined in open type dual-roller cylinder refining glue at room temperature, and silicone rubber compounds are added to roller first
On, after sizing material packet roller of machining, it is gradually added reinforced filling, ageing-resistant additive, coupling agent；Sizing material after being kneaded uniformly is thin
After logical 8 ~ 10 times, clot bottom sheet, obtain rubber compound deposit in it is spare in drier；Rubber compound carries out back mixing after placing 24 hours,
It is carried out on open type dual-roller cylinder rubber mixing machine, when sizing material limbers up, surface is smooth, Bao Tong 5 ~ 10 times, can blanking slice；
Then by silicon rubber gross rubber on open type dual-roller cylinder rubber mixing machine packet roller, be added crosslinking agent, catalyst, 10 left sides Bao Tong
The right side, by blob of viscose on two roller machine slice；Pressing force container model requirement prepares capsule die, then by silicon rubber raw cook packet in glue
On capsule mold, by shaping, calendering overlap edge process, capsule size is made to meet the requirements, and in silicon rubber top covering cloth, fixed silicon
Rubber raw rubber capsule, carries out one step cure under normal pressure, and heat transfer medium is hot-air, and curing temperature is 160 ~ 170 DEG C, when vulcanization
Between about 20min；The capsule of different piece is finally bonded together carry out post vulcanization by adhesive.
3. a kind of method for preparing solid propellant rocket liner molding silicone rubber air capsule material as claimed in claim 2,
It is characterized in that, by blob of viscose on two roller machine slice with a thickness of 2mm.
4. a kind of method for preparing solid propellant rocket liner molding silicone rubber air capsule material as claimed in claim 2,
It is characterized in that, the capsule die is fabricated separately according to head, tail portion, shell portion.
5. a kind of method for preparing solid propellant rocket liner molding silicone rubber air capsule material as claimed in claim 2,
It is characterized in that, the condition of the post vulcanization is at 150 DEG C, the progress time is 120min.
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Families Citing this family (4)
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| CN108329604B (en) * | 2018-01-29 | 2021-04-13 | 湖北华强科技股份有限公司 | Formula and preparation method of rubber air bag for liquid bomb |
| CN111086128A (en) * | 2019-12-27 | 2020-05-01 | 湖北航聚科技有限公司 | Core mold for manufacturing solid rocket engine and forming method thereof |
| CN112318790B (en) * | 2020-09-09 | 2022-08-19 | 西安近代化学研究所 | Vulcanization molding process for high-viscosity silicon-based heat insulation layer |
| CN114933803A (en) * | 2021-09-03 | 2022-08-23 | 安徽立航复合材料科技有限公司 | High-hardness silicone rubber air bag for curing heat insulation layer of solid rocket engine |
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