CN109135073A - A kind of resistance to ablation ternary ethlene propyene rubbercompound material and preparation method thereof - Google Patents
A kind of resistance to ablation ternary ethlene propyene rubbercompound material and preparation method thereof Download PDFInfo
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- CN109135073A CN109135073A CN201811001907.4A CN201811001907A CN109135073A CN 109135073 A CN109135073 A CN 109135073A CN 201811001907 A CN201811001907 A CN 201811001907A CN 109135073 A CN109135073 A CN 109135073A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention provides a kind of ternary ethlene propyene rubbercompound materials of resistance to ablation and preparation method thereof, belong to field of high polymer material modification, the composite material has excellent ablation resistance and mechanical property using ethylene propylene diene rubber as matrix, by adding the ternary ethlene propyene rubbercompound material that fire retardant trapezoidal polyphenyl base vinyl silsesquioxane makes.Embodiment experimental data shows the linear ablative rate of the ternary ethlene propyene rubbercompound material of resistance to ablation provided by the invention up to 0.116mm/s, and carbonization degree is up to 0.2321mm/s.
Description
Technical field
The present invention relates to field of high polymer material modification, in particular to a kind of ethylene propylene diene rubber of resistance to ablation composite wood
Material and preparation method thereof.
Background technique
Interior heat-insulating material is the important component of solid propellant rocket and propellant loading, be located at motor body with
Between solid propellant.The important function of interior heat-insulating material is exactly high temperature, high combustion gas stream and particle in solid propellant rocket
Under object erosion-corrosion environment, do not lose it is strong, do not burn, prevent motor combustion chamber case from reaching and jeopardize self structure integrality temperature, from
And guarantee the normal work of solid propellant rocket.Ethylene propylene diene rubber (EPDM) is ethylene, propylene and non-conjugated diene hydrocarbon
Terpolymer, be low unsaturated rubber, main chain saturation, branch is unsaturated.Its density is minimum in all rubber, and
It can achieve ideal mechanical property and ablation property by the cooperation of suitable auxiliary agents.Therefore, the EPDM since the seventies
Rubber heat-insulating material obtains very big development, and application range is also increasingly wider.Since rubber base material itself is unable to satisfy
The environmental requirement that high temperature, high pressure, high-speed flow wash away in Solid Rocket Motor combustion chamber, therefore in the prior art, it can add
Enter scour resistance and resistance to burning of the various fillers such as silica, powdered phenol-formaldehyde resin, ammonium polyphosphate to improve interior heat-insulating material
Corrosion.But the research with more novel propellants with the development of science and technology, the operating temperature and pressure of combustion chamber will also be into one
Step improves, therefore it is imperative to obtain the more superior interior heat-insulating material of ablation resistance.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of ternary ethlene propyene rubbercompound material of resistance to ablation and its preparation sides
Method, the ternary ethlene propyene rubbercompound material of resistance to ablation provided by the invention have excellently ablation resistance.
The present invention provides a kind of ternary ethlene propyene rubbercompound materials of resistance to ablation, by the raw material system including following mass fraction
It is standby to obtain:
The fire retardant includes the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I；
In Formulas I, the ratio of m and n are 10:1~100；
The filler of resistance to ablation is silica and phenolic resin；
The synergy resin is terpene resin and/or chlorosulfonated polyethylene.
Preferably, the fire retardant further includes time diethyl hypo-aluminum orthophosphate.
Preferably, the quantity of phenyl and vinyl ratio is 9~1:1 in the trapezoidal polyphenyl base vinyl silsesquioxane.
Preferably, the fiber of resistance to ablation is Fanglun slurry cake, polyparaphenylene's benzo twoport oxazole fiber or F12Aramid fiber is fine
Dimension.
Preferably, the activator is zinc oxide and stearic acid.
Preferably, the silane coupling agent is double-[γ-(triethoxysilicane) propyl] tetrasulfide and/or γ-aminopropyl
Triethoxysilane.
Preferably, the promotor is -2. benzothiazole sulfenamide of N- cyclohexyl and/or diphenylguanidine.
Preferably, the vulcanizing agent is sulphur and/or cumyl peroxide.
The present invention also provides the preparation methods of above-mentioned composite material, comprising the following steps:
Ethylene propylene diene rubber is successively even with plasticizing aid, the fiber of resistance to ablation, activator, fire retardant, synergy resin, silane
Connection agent, the filler of resistance to ablation, promotor and vulcanizing agent carry out mixing of plasticating, and obtain broken-down rubber；
By the broken-down rubber successively at base, be stored at room temperature and vulcanize, obtain the ternary ethlene propyene rubbercompound material of resistance to ablation.
Preferably, the temperature of the vulcanization is 160~170 DEG C, and the time of vulcanization is 30~60min, and the pressure of vulcanization is
10~15MPa.
Advantageous effects: the present invention provides a kind of ternary ethlene propyene rubbercompound material of resistance to ablation and preparation method thereof,
The composite material makes to obtain using ethylene propylene diene rubber as matrix by adding fire retardant trapezoidal polyphenyl base vinyl silsesquioxane
Ternary ethlene propyene rubbercompound material have excellent ablation resistance and mechanical property.Embodiment experimental data shows this hair
For the linear ablative rate of the ternary ethlene propyene rubbercompound material of resistance to ablation of bright offer up to 0.116mm/s, carbonization degree is reachable
0.2321mm/s。
Specific embodiment
The present invention provides a kind of ternary ethlene propyene rubbercompound materials of resistance to ablation, by the raw material system including following mass fraction
It is standby to obtain:
The fire retardant includes the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I；
In Formulas I, the ratio of m and n are 10:1~100；
The filler of resistance to ablation is silica and phenolic resin；
The synergy resin is terpene resin and/or chlorosulfonated polyethylene.
In the present invention, the fire retardant includes the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I.
In the present invention, the preparation method of the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I
The following steps are included:
Phenyl silane, vinyl silanes and organic solvent are mixed, mixed solution is obtained；
To the mixed solution and dripping catalyst aqueous solution, hydrolysis occurs, obtains hydrolysate；
The hydrolysate is heated up, copolycondensation occurs, obtains copolycondensation product；
White solid is precipitated after the copolycondensation product is mixed with alcohols solvent, obtains the ladder with structure shown in Formulas I
Shape polyphenylethylene base silsesquioxane, the alcohols solvent are dehydrated alcohol or anhydrous methanol.
The present invention mixes phenyl silane, vinyl silanes and organic solvent, obtains mixed solution.In the present invention, institute
The molar ratio for stating phenyl silane and vinyl silanes is preferably 10:1~10:100.
In the present invention, the volume ratio of the gross mass and organic solvent of the phenyl silane and vinyl silanes is preferably
1g:5~50mL.
In the present invention, the phenyl silane is preferably three second of phenyl trichlorosilane, phenyltrimethoxysila,e or phenyl
Oxysilane.
In the present invention, the vinyl silanes are preferably vinyl trichlorosilane, vinyltrimethoxysilane or second
Alkenyl triethoxysilane.
In the present invention, the organic solvent is preferably acetone, petroleum ether, acetonitrile, methylene chloride, chloroform, tetrahydro
One of furans, pyridine and dioxane are a variety of.
After obtaining mixed solution, the present invention occurs hydrolysis, obtains to the mixed solution and dripping catalyst aqueous solution
To hydrolysate.In the present invention, the catalyst preferably includes potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate, tetramethyl
One of base ammonium hydroxide and tetraethyl ammonium hydroxide are a variety of.When the catalyst is preferably mixture, the present invention couple
The mass ratio of substance does not have special restriction in the catalyst, using the mixture of any mass ratio.
In the present invention, the rate of the dropwise addition is preferably added dropwise.
In the present invention, the mass ratio of the gross mass and catalyst of the phenyl silane and vinyl silanes is preferably 1:
0.005~0.1, the quality of catalyst and the volume ratio of water are preferably 1g:50~200mL in the catalyst aqueous solution.
In the present invention, the hydrolysis preferably carries out at normal temperatures and pressures, does not need additional heating or cooling.?
In hydrolytic process, the phenyl silane and vinyl silanes generate silanol.
After obtaining hydrolysate, the present invention, which heats up the hydrolysate, occurs copolycondensation, obtains copolycondensation product.
In the present invention, the temperature of the copolycondensation is preferably 40~80 DEG C, and more preferably 60~70 DEG C, the copolycondensation
Time be preferably 12~72h, more preferably 24~36h.
The present invention does not have special restriction to the heating rate of the heating, using heating well known to those skilled in the art
Rate.
After obtaining copolycondensation product, white solid is precipitated after mixing the copolycondensation product with alcohols solvent in the present invention,
The trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I is obtained, the alcohols solvent is dehydrated alcohol or anhydrous
Methanol.
In the present invention, the volume ratio of the copolycondensation product and alcohols solvent is preferably 1:5~50.
After white solid is precipitated, the present invention is preferably successively filtered, distills washing, ethanol washing and drying, is had
The trapezoidal polyphenyl base vinyl silsesquioxane of structure shown in Formulas I.The present invention is to the suction filtration, distillation washing and ethanol washing
Concrete mode does not have special restriction, using mode well known to those skilled in the art.
In the present invention, the temperature of the drying is preferably 60~120 DEG C, and more preferably 80 DEG C, the time of the drying
Preferably 8~12h, more preferably 10h.
In the present invention, phenyl and second in the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I
The quantity of alkenyl is than being preferably 9~1:1, more preferably 7~3:1, most preferably 5:1.
In the present invention, the fire retardant further includes diethyl hypo-aluminum orthophosphate and/or zinc borate.When the fire retardant is two
When ethyl hypo-aluminum orthophosphate and trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I, the diethyl hypophosphorous acid
The mass ratio of aluminium and the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I is preferably 10~1:1, more preferably
6~3:1；When the fire retardant is zinc borate and trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I, institute
The mass ratio for stating zinc borate and the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I is preferably 1:15~2:1,
More preferably 4:15~4:5；When fire retardant is diethyl hypo-aluminum orthophosphate, zinc borate and the trapezoidal polyphenyl base for having structure shown in Formulas I
When vinyl silsesquioxane, the diethyl hypo-aluminum orthophosphate, zinc borate and the trapezoidal polyphenyl base vinyl for having structure shown in Formulas I
The mass ratio of silsesquioxane is preferably 12~1:1, more preferably 7~2:1.
In the present invention, the mass fraction of the fire retardant is preferably 30~60 parts, and more preferably 45 parts.
In the present invention, the filler of resistance to ablation is silica and phenolic resin.
In the present invention, the mass ratio of the silica and phenolic resin is preferably 2~0.5:1, more preferably 1:1.
In the present invention, the mass fraction of the filler of resistance to ablation is preferably 40~55 parts, and more preferably 40~50 parts.
In the present invention, the synergy resin is terpene resin and/or chlorosulfonated polyethylene.
In the present invention, when the synergy resin is terpene resin and chlorosulfonated polyethylene, the terpene resin and chlorine sulphur
The mass ratio for changing polyethylene is preferably 2~0.5:1, more preferably 1:1.
In the present invention, the mass fraction of the synergy resin is preferably 10~15 parts.
In the present invention, the fiber of resistance to ablation is preferably Fanglun slurry cake, polyparaphenylene's benzo twoport oxazole fiber or F12-
Aramid fiber.
In the present invention, the mass fraction of the fiber of resistance to ablation is preferably 6~8 parts.
In the present invention, the plasticizing aid is preferably paraffin oil.
In the present invention, the activator is preferably zinc oxide and stearic acid.
In the present invention, the mass fraction of the activator is preferably 6~8 parts.
In the present invention, the silane coupling agent preferably double-[γ-(triethoxysilicane) propyl] tetrasulfide and/or
Or mixtures thereof gamma-aminopropyl-triethoxy-silane.
In the present invention, the promotor is preferably -2. benzothiazole sulfenamide of N- cyclohexyl and/or diphenylguanidine.When
When promotor is -2. benzothiazole sulfenamide of N- cyclohexyl and diphenylguanidine, the present invention is to N- cyclohexyl -2. benzothiazole time sulphur
The mass ratio of amide and diphenylguanidine is not particularly limited, and is mixed with arbitrary proportion.
In the present invention, the mass fraction of the promotor is preferably 1.5~4 parts, and more preferably 2.5 parts.
In the present invention, the vulcanizing agent is preferably sulphur and/or cumyl peroxide.When the vulcanizing agent is sulphur
And cumyl peroxide, the present invention is not particularly limited the mass ratio of sulphur and cumyl peroxide, with arbitrary proportion
Mixing.
The present invention also provides the preparation methods of above-mentioned composite material, comprising the following steps:
Ethylene propylene diene rubber is successively even with plasticizing aid, the fiber of resistance to ablation, activator, fire retardant, synergy resin, silane
Connection agent, the filler of resistance to ablation, promotor and vulcanizing agent carry out mixing of plasticating, and obtain broken-down rubber；
By the broken-down rubber successively at base, be stored at room temperature and vulcanize, obtain the ternary ethlene propyene rubbercompound material of resistance to ablation.
The present invention by ethylene propylene diene rubber successively with plasticizing aid, the fiber of resistance to ablation, activator, fire retardant, synergy resin,
Silane coupling agent, the filler of resistance to ablation, promotor and vulcanizing agent carry out mixing of plasticating, and obtain broken-down rubber.
In the present invention, it after each raw material is added, first plasticates uniformly mixed, adds next raw material.For example, by ternary
EP rubbers and plasticizing aid are plasticated after mixing, add fire retardant plasticate it is uniformly mixed, and so on.
In the present invention, the plasticizing aid is conducive to ethylene propylene diene rubber rubber bag roller, so being added at first；It is described resistance to
Ablation fiber is more early added to increase jitter time；The filler of resistance to ablation is added after silane coupling agent is conducive to its point
It dissipates, and improves rubbery intensity, vulcanizing agent, which is eventually adding, prevents matrix from crosslinking solidification in mixing process.
After obtaining broken-down rubber, the present invention by the broken-down rubber successively at base, be stored at room temperature and vulcanize, obtain resistance to ablation ternary
EP rubbers composite material.
The present invention is not particularly limited at the method for base, selects the known ground of those skilled in the art at blank technology.
In the present invention, the time being stored at room temperature be preferably 16~for 24 hours, more preferably 18~20h, relaxation rubber is big
Molecule builds up structural fatigue due to the effect by external mechanical force in mixing process, and is moulding for various additives
The further evenly dispersed offer time in refining glue completes the dispersion process for having little time completion in plasticating.
In the present invention, the temperature of the vulcanization is preferably 160~170 DEG C, and more preferably 160~165 DEG C；The vulcanization
Time be preferably 30~60min, the pressure of more preferably 40~55min, most preferably 45~50min, the vulcanization are preferred
For 10~15MPa, more preferably 15MPa.
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
The preparation of trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I
1) by 17.33g phenyltrimethoxysila,e and 2.38g vinyltriethoxysilane (the two molar ratio is 7:1)
It is added in the 500mL three-necked flask with reflux condensing tube, constant pressure funnel, temperature regulating device and magnetic agitation, is added
0.1g KOH, is then dissolved in 10mL distilled water, the aqueous solution of KOH is slowly dropped to three mouthfuls of burnings by 200mL acetone, stirring
In bottle, about 30min is dripped off, and 60 DEG C are warming up to after being added dropwise, and is reacted 12h, is obtained faint yellow reaction solution.
2) under agitation, the obtained reaction solution of step 1) is poured into the dehydrated alcohol of 3L, stirs 30min,
It is then allowed to stand about 1h, the solution of the colorless and transparent lower layer's white precipitate in upper layer is obtained, this solution is filtered, with distilled water and anhydrous second
Alcohol washs three times repeatedly, and filter cake is placed in drying 10 hours in 60 DEG C of vacuum drying ovens, finally obtains the ladder with structure shown in Formulas I
Shape polyphenylethylene base silsesquioxane.
The raw materials and consumption (mass fraction) for the ternary ethlene propyene rubbercompound material of resistance to ablation:
100 parts of ethylene propylene diene rubber
5 parts of paraffin oil
7 parts of Fanglun slurry cake
5 parts of zinc oxide
1 part of stearic acid
4 parts of zinc borate
30 parts of diethyl hypo-aluminum orthophosphate
Above-mentioned 5 parts of the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I being prepared
5 parts of terpene resin
5 parts of chlorosulfonated polyethylene
Double -5 parts of tetrasulfide of [γ-(triethoxysilicane) propyl]
20 parts of silica
20 parts of boron bakelite resin
2 parts of -2. benzothiazole sulfenamide of N- cyclohexyl
0.5 part of diphenylguanidine
4 parts of cumyl peroxide
0.8 part of sulphur
The preparation method for the ternary ethlene propyene rubbercompound material of resistance to ablation:
1) ethylene propylene diene rubber is plasticated on the double roll mill with paraffin oil and is uniformly mixed, obtain mixture I；It is mixing
Fanglun slurry cake is added in material I, then plasticates uniformly mixed, obtains mixture II；Sequentially added in mixture II zinc oxide and
Stearic acid is plasticated uniformly mixed, and mixture III is obtained；Zinc borate, diethyl hypo-aluminum orthophosphate are sequentially added in mixture III
(ADP) and trapezoidal polyphenyl base vinyl silsesquioxane it, plasticates uniformly mixed, obtains mixture IV；Successively add in mixing IV
Enter terpene resin and chlorosulfonated polyethylene, plasticate uniformly mixed, obtains mixture V；Double-[γ-(three second are added in mixture V
Oxygroup silicon) propyl] tetrasulfide, it plasticates uniformly mixed, obtains mixture VI；Silica and boron phenol are added in mixture VI
Urea formaldehyde is plasticated uniformly mixed, and mixture VII is obtained；- 2. benzothiazole of N- cyclohexyl is sequentially added in mixture VII
Sulfonamide (CZ) and diphenylguanidine (D), then plasticate uniformly mixed, obtain mixture VIII；It is sequentially added in mixture VIII
Then cumyl peroxide and sulphur plasticate uniformly mixed, obtain broken-down rubber.
2) broken-down rubber obtained in step 1) is prefabricated into blank material by mold shape, is carried out after placing 16 hours at room temperature
Vulcanization obtains the ternary ethlene propyene rubbercompound material of resistance to ablation containing trapezoidal polyphenyl base vinyl silsesquioxane；Curing temperature
160 DEG C, the time is 45 minutes, pressure 15MPa.
Embodiment 2
The quality for the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I being prepared in embodiment 1
Number is 10 parts, and type, dosage and the preparation method of other raw materials are identical with embodiment 1.Obtain resistance to ablation ternary second
Third rubber composite material.
Embodiment 3
The quality for the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I being prepared in embodiment 1
Number is 15 parts, and type, dosage and the preparation method of other raw materials are identical with embodiment 1.Obtain resistance to ablation ternary second
Third rubber composite material.
Embodiment 4
The quality for the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I being prepared in embodiment 1
Number is 15 parts, and the mass fraction of aluminum diethylphosphinate is 40 parts, type, dosage and the preparation method and reality of other raw materials
It is identical to apply example 1.Obtain the ternary ethlene propyene rubbercompound material of resistance to ablation.
Embodiment 5
Without the trapezoidal polyphenyl base vinyl silsesquioxane being prepared in embodiment 1 with structure shown in Formulas I with
Chlorosulfonated polyethylene, type, dosage and the preparation method of other raw materials are identical with embodiment 1.Obtain resistance to ablation ternary
EP rubbers composite material.
Comparative example 1
Without containing the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I is prepared in embodiment 1,
Type, dosage and the preparation method of other raw materials are identical with embodiment 1.Obtain ternary ethlene propyene rubbercompound material.
The ternary ethlene propyene rubbercompound material of resistance to ablation that Examples 1 to 4 is obtained carries out mechanical property and ablation experiments are surveyed
Examination.
Mechanics Performance Testing condition are as follows: tested using Shanghai moral outstanding person's DXLL-5000 type electronic tension tester.It presses
GB/T528-2009 measurement, dumbbell-shaped specimen, tensile speed 200mm/min, temperature is room temperature.
Ablation experiments test condition are as follows: use oxy-acetylene ablation test device, carried out by GJB323A-96, ablation distance
For 10mm, ablation time 20s, nozzle diameter 2mm, oxygen flow 0.42m3/ s, acetylene flow 0.31m3/ s, linear ablative rate can tables
It is shown as: linear ablative rate=(residual thickness of the original thickness-containing layer of charcoal)/ablation time
Test result are as follows: the tensile strength of the resistance to composite material of the ethylene propylene diene rubber of resistance to ablation is 9.5MPa in embodiment 1, is broken
Splitting elongation is 71%, linear ablative rate 0.119mm/s, carbonization degree 0.2321mm/s；Resistance to ablation EPDM in embodiment 2
The tensile strength of the resistance to composite material of rubber is 9.3MPa, and elongation at break 74%, linear ablative rate 0.131mm/s, carbonization degree is
0.2334mm/s；The tensile strength of the resistance to composite material of the ethylene propylene diene rubber of resistance to ablation is 4.1MPa, elongation at break in embodiment 3
It is 287%, linear ablative rate 0.116mm/s, carbonization degree 0.2327mm/s.The ethylene propylene diene rubber of resistance to ablation is resistance in embodiment 4
The tensile strength of composite material is 3.8MPa, and elongation at break 265%, linear ablative rate 0.109mm/s, carbonization degree is
0.2289mm/s；The tensile strength of the resistance to composite material of the ethylene propylene diene rubber of resistance to ablation is 4MPa in embodiment 5, and elongation at break is
211%, linear ablative rate 0.138mm/s, carbonization degree 0.2458mm/s；Ethylene propylene diene rubber obtained in comparative example 1 is resistance to multiple
Condensation material tensile strength is 4.1MPa, and elongation at break 358%, linear ablative rate 0.134mm/s, carbonization degree is
0.2335mm/s。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of ternary ethlene propyene rubbercompound material of resistance to ablation is prepared by the raw material for including following mass fraction:
The fire retardant includes the trapezoidal polyphenyl base vinyl silsesquioxane with structure shown in Formulas I；
In Formulas I, the ratio of m and n are 10:1~100；
The filler of resistance to ablation is silica and phenolic resin；
The synergy resin is terpene resin and/or chlorosulfonated polyethylene.
2. composite material according to claim 1, which is characterized in that the fire retardant further includes diethyl hypo-aluminum orthophosphate
And/or zinc borate.
3. composite material according to claim 1 or 2, which is characterized in that the trapezoidal polyphenyl base vinyl silicon sesquialter oxygen
The quantity of phenyl and vinyl ratio is 9~1:1 in alkane.
4. composite material according to claim 1, which is characterized in that the fiber of resistance to ablation is Fanglun slurry cake, gathers to benzene
Support benzo twoport oxazole fiber or F12Aramid fiber.
5. composite material according to claim 1, which is characterized in that the activator is zinc oxide and stearic acid.
6. composite material according to claim 1, which is characterized in that the silane coupling agent is double-[γ-(triethoxy
Silicon) propyl] or mixtures thereof tetrasulfide and/or gamma-aminopropyl-triethoxy-silane.
7. composite material according to claim 1, which is characterized in that the promotor is -2. benzothiazole of N- cyclohexyl
Sulfenamide and/or diphenylguanidine.
8. composite material according to claim 1, which is characterized in that the vulcanizing agent is that sulphur and/or peroxidating two are different
Propyl benzene.
9. the preparation method of composite material described in claim 1~8 any one, comprising the following steps:
By ethylene propylene diene rubber successively with the plasticizing aid, fiber of resistance to ablation, activator, fire retardant, synergy resin, silane coupled
Agent, the filler of resistance to ablation, promotor and vulcanizing agent carry out mixing of plasticating, and obtain broken-down rubber；
By the broken-down rubber successively at base, be stored at room temperature and vulcanize, obtain the ternary ethlene propyene rubbercompound material of resistance to ablation.
10. preparation method according to claim 9, which is characterized in that the temperature of the vulcanization is 160~170 DEG C, vulcanization
Time be 30~60min, the pressure of vulcanization is 10~15MPa.
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| CN113290997A (en) * | 2021-05-28 | 2021-08-24 | 北京理工大学 | Surface-compounded thermal protection material and preparation method thereof |
| CN113321875A (en) * | 2021-05-27 | 2021-08-31 | 北京理工大学 | Organic-inorganic composite thermal protection and heat insulation material and preparation method thereof |
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| CN113321875A (en) * | 2021-05-27 | 2021-08-31 | 北京理工大学 | Organic-inorganic composite thermal protection and heat insulation material and preparation method thereof |
| CN113290997A (en) * | 2021-05-28 | 2021-08-24 | 北京理工大学 | Surface-compounded thermal protection material and preparation method thereof |
| CN117384449A (en) * | 2023-09-20 | 2024-01-12 | 西安理工大学 | Hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat insulation material as well as preparation method and application thereof |
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