CN102120849B - Ethylene-propylene-diene monomer (EPDM) ablation-resistant composition containing high-regularity trapezoid polyphenyl silsesquioxane and preparation method thereof - Google Patents
Ethylene-propylene-diene monomer (EPDM) ablation-resistant composition containing high-regularity trapezoid polyphenyl silsesquioxane and preparation method thereof Download PDFInfo
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- CN102120849B CN102120849B CN201010606018A CN201010606018A CN102120849B CN 102120849 B CN102120849 B CN 102120849B CN 201010606018 A CN201010606018 A CN 201010606018A CN 201010606018 A CN201010606018 A CN 201010606018A CN 102120849 B CN102120849 B CN 102120849B
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- 238000002679 ablation Methods 0.000 title claims abstract description 41
- 239000000203 mixture Substances 0.000 title claims abstract description 23
- 229920006389 polyphenyl polymer Polymers 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920002943 EPDM rubber Polymers 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 9
- 239000003063 flame retardant Substances 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 6
- 229920001971 elastomer Polymers 0.000 claims description 45
- 229920001897 terpolymer Polymers 0.000 claims description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- KBXJHRABGYYAFC-UHFFFAOYSA-N octaphenylsilsesquioxane Chemical compound O1[Si](O2)(C=3C=CC=CC=3)O[Si](O3)(C=4C=CC=CC=4)O[Si](O4)(C=5C=CC=CC=5)O[Si]1(C=1C=CC=CC=1)O[Si](O1)(C=5C=CC=CC=5)O[Si]2(C=2C=CC=CC=2)O[Si]3(C=2C=CC=CC=2)O[Si]41C1=CC=CC=C1 KBXJHRABGYYAFC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract 2
- 239000004114 Ammonium polyphosphate Substances 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 abstract 2
- 229920001276 ammonium polyphosphate Polymers 0.000 abstract 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229920000137 polyphosphoric acid Polymers 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 4
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 4
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 3
- 229920001342 Bakelite® Polymers 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 239000004637 bakelite Substances 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- GPNLWUFFWOYKLP-UHFFFAOYSA-N s-(1,3-benzothiazol-2-yl)thiohydroxylamine Chemical group C1=CC=C2SC(SN)=NC2=C1 GPNLWUFFWOYKLP-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- UQSHIDHNLKIYGN-UHFFFAOYSA-N diphenoxyphosphoryl diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OP(=O)(OC=1C=CC=CC=1)OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 UQSHIDHNLKIYGN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009421 internal insulation Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to an ethylene-propylene-diene monomer (EPDM) ablation-resistant composition containing high-regularity trapezoid polyphenyl silsesquioxane and a preparation method thereof, belonging to the technical field of heat insulation and ablation resistance. With EPDM as a substrate, the composition also comprises a plasticizing aid, ablation-resistant fibers, an activating agent, flame retardant, ablation-resistant fillers, an accelerating agent, a vulcanizing agent and a silane coupling agent. The preparation method comprises the following steps of: uniformly plasticating and mixing the EPDM and the plasticizing aid, the ablation-resistant fibers, the activating agent, the flame retardant, the ablation-resistant fillers, the accelerating agent, the vulcanizing agent and the silane coupling agent in sequence on a dual-roller open mill, prefabricating into a blank material according to the shape of a die, standing for 16-24h under a room temperature and then vulcanizing for 45-60 minutes at a vulcanizing temperature of 160-170 DEG C under the pressure of 10-15MPa to obtain the EPDM ablation-resistant composition containing the high-regularity trapezoid polyphenyl silsesquioxane. In the invention, through adding ammonium polyphosphate and the trapezoid polyphenyl silsesquioxane and optimizing the contents of the ammonium polyphosphate and the trapezoid polyphenyl silsesquioxane, the material obtained by adopting the preparation method provided by the invention has a low ablation effect and favorable mechanical properties.
Description
Technical field
The present invention relates to terpolymer EP rubber mixture of anti-ablation that contains the high-tacticity trapezoidal polyphenyl silicious sesquioxane and preparation method thereof, belong to heat insulation anti-ablation technology field.
Background technology
The main effect of thermal insulation material is that housing is played heat-blocking action, reaches the temperature that jeopardizes its structural integrity in order to prevent housing.
The density of terpolymer EP rubber (EPDM) minimum in all rubber, and can reach ideal mechanical property and ablation property through the cooperation of suitable auxiliary agents, therefore, the anti-ablation of terpolymer EP rubber was developed on a large scale from the seventies very much.But, along with the expansion that the development of technology and thermal insulation material are used, the internal insulation of protection housing is had higher requirement, antiscour, anti-ablation, performance such as high pressure resistant is the demand direction to ablator.
Rubber can form cross-linked network through vulcanizing agent, provides material to use required mechanical strength and unit elongation.Because rubber base material itself can't satisfy the environmental requirement that high temperature, high pressure, high velocity air wash away in the Solid Rocket Motor combustion chamber, therefore must add the various fillers of anti-the ablation to improve its antiscour, ablation resistance.Exploitation novel, fire retardant efficiently and composite makes that the degraded of body material is slower; The introducing of the novel filler of anti-the ablation improves high temperature resistant, the erosion resistibility of material greatly.
The structure of ladder-like poly-phenyl silsesquioxane and preparation method see patent " a kind of preparation method of high-tacticity trapezoidal polyphenyl silicious sesquioxane " among the present invention, and its patent No. is 201010190169.X.
Summary of the invention
The present invention seeks to can keep under the situation of better mechanical property in order to provide a kind of, the thermal insulation material that its ablation resistance is good proposes a kind of terpolymer EP rubber mixture of anti-ablation that contains the high-tacticity trapezoidal polyphenyl silicious sesquioxane and preparation method thereof.
The terpolymer EP rubber mixture of anti-ablation that contains the high-tacticity trapezoidal polyphenyl silicious sesquioxane of the present invention as matrix, and is 100 parts in terpolymer EP rubber with terpolymer EP rubber, and other components contents are:
5 parts of plasticizing auxiliary agents
5～10 parts of the fibers of anti-the ablation
6～10 parts in acvator
20～90 parts of fire retardants
40～60 parts of the fillers of anti-the ablation
1.5～6 parts of promotor
4～6 parts of vulcanizing agents
4 parts of silane coupling agents
Wherein, the plasticizing auxiliary agent is a Yellow Protopet 2A; The fiber of anti-the ablation is polyterephthalamide Ursol D (PPTA) short fiber or pulp; Acvator comprises zinc oxide, also can add Triple Pressed Stearic Acid in the acvator; Fire retardant comprises polyphosphoric acid amine (APP) and ladder-like poly-phenyl silsesquioxane, in fire retardant, can also add in triphenylphosphate (TPP), polyphosphoric acid melamine (MPP), metaphenylene tetraphenyl diphosphate (RDP), the zinc borate one or more; The filler of anti-the ablation comprises silicon-dioxide or boron bakelite resin, can also add in sepiolite, ceramic fine bead, the glass microballon one or more in the filler of anti-the ablation; Promotor is benzothiazole sulphenamide (CZ), vulkacit D (D) or its mixture of N-cyclohexyl-2.; Vulcanizing agent is sulphur, Di Cumyl Peroxide 99 or its mixture; Silane coupling agent is two-(3-triethoxyl silane propyl group)-tetrasulfide, γ-An Bingjisanyiyangjiguiwan or its mixture.
The preparation method who contains the terpolymer EP rubber mixture of anti-ablation of high-tacticity trapezoidal polyphenyl silicious sesquioxane of the present invention, its concrete preparation process is:
1) in two roller mills, terpolymer EP rubber and plasticizing auxiliary agent are plasticated and mixed;
2) 1) in terpolymer EP rubber in add the fiber of anti-the ablation, plasticating then mixes;
3) 2) in terpolymer EP rubber in add acvator, plasticating then mixes;
4) 3) in terpolymer EP rubber in add fire retardant, plasticating then mixes;
5) 4) in terpolymer EP rubber in add the filler of anti-the ablation, plasticating then mixes;
6) 5) in terpolymer EP rubber in add promotor, plasticating then mixes;
7) 6) in terpolymer EP rubber in add vulcanizing agent and silane coupling agent, plasticating then mixes;
8) with 7) in the mixture that mixes of plasticating be prefabricated into the base material by mold shape;
9) with 8) in the base material at room temperature place and vulcanize the terpolymer EP rubber mixture of anti-ablation that obtains containing the high-tacticity trapezoidal polyphenyl silicious sesquioxane after 16～24 hours; Curing temperature is 160～170 ℃, and the time is 45～60 minutes, and pressure is 10～15MPa.
Beneficial effect
The present invention makes the material that obtains reach low effect and its good mechanical properties of ablating through adding the optimization of polyphosphoric acid amine and ladder-like poly-phenyl silsesquioxane and both content.
Embodiment
Embodiment
As material matrix, and is 100 parts in terpolymer EP rubber with terpolymer EP rubber, and other components contents are:
5 parts of Yellow Protopet 2As
6 parts of PPTA pulps
5 parts in zinc oxide
1 part of Triple Pressed Stearic Acid
30 parts of polyphosphoric acid amine (APP)
10 parts of ladder-like poly-phenyl silsesquioxanes
4 parts of zinc borates (ZB)
20 parts of silicon-dioxide
20 parts of boron bakelite resins
2 parts of the benzothiazole sulphenamides (CZ) of N-cyclohexyl-2.
0.5 part of vulkacit D (D)
0.8 part in sulphur
4 parts of Di Cumyl Peroxide 99s
4 parts of γ-An Bingjisanyiyangjiguiwans
1) in two roller mills, terpolymer EP rubber and Yellow Protopet 2A plasticated and mix;
2) 1) in terpolymer EP rubber in add the PPTA pulp, plasticating then mixes;
3) 2) in terpolymer EP rubber in add zinc oxide and Triple Pressed Stearic Acid, plasticating then mixes:
4) 3) in terpolymer EP rubber in add polyphosphoric acid amine (APP), ladder-like poly-phenyl silsesquioxane and zinc borate, plasticating then mixes;
5) 4) in terpolymer EP rubber in add silicon-dioxide and boron bakelite resin, plasticating then mixes;
6) 5) in terpolymer EP rubber in add N-cyclohexyl-2. benzothiazole sulphenamide (CZ) and vulkacit D (D), plasticating then mixes;
7) 6) in terpolymer EP rubber in add sulphur, Di Cumyl Peroxide 99 and γ-An Bingjisanyiyangjiguiwan, plasticating then mixes;
8) with 7) in the mixture that mixes of plasticating be prefabricated into square base material by mold shape;
9) with 8) in the base material at room temperature place to vulcanize after 17 hours and obtain the terpolymer EP rubber mixture of anti-the ablation; Curing temperature is 170 ℃, and the time is 60 minutes, and pressure is 15MPa.
The terpolymer EP rubber mixture of anti-ablation that aforesaid method is obtained carries out mechanical property and ablation experiments test.
The Mechanics Performance Testing condition is: adopt the outstanding DXLL-5000 type of Shanghai moral electronic tension tester to test.Press GB/T528-92 and measure dumbbell-shaped specimen, draw speed 500mm/min, 20 ℃ of temperature.
The ablation experiments test condition is: adopt oxy-acetylene ablation test device, undertaken by GJB323A-96, the distance of ablating is 10mm, the time 20s that ablates, nozzle diameter 2mm, oxygen 0.42m
3/ s, acetylene 0.31m
3/ s.
The tensile strength of the terpolymer EP rubber mixture of anti-ablation that contains the high-tacticity trapezoidal polyphenyl silicious sesquioxane that test obtains is 9.38MPa, and elongation at break is 375%, and carbonization degree is 0.127mm/s.
Comparative Examples
With embodiment 1, the difference is that not add ladder-like poly-phenyl silsesquioxane, the tensile strength that obtains at last is 10.93MPa, and elongation at break is 332%, and the carbonization degree of terpolymer EP rubber is 0.173mm/s.
Claims (2)
1. contain the terpolymer EP rubber mixture of anti-ablation of high-tacticity trapezoidal polyphenyl silicious sesquioxane, it is characterized in that: is 100 parts in terpolymer EP rubber as matrix and with terpolymer EP rubber, and other components contents are:
2. described preparation method who contains the terpolymer EP rubber mixture of anti-ablation of high-tacticity trapezoidal polyphenyl silicious sesquioxane of claim 1 is characterized in that concrete preparation process is:
1) in two roller mills, terpolymer EP rubber and plasticizing auxiliary agent are plasticated and mixed;
2) 1) in terpolymer EP rubber in add the fiber of anti-the ablation, plasticating then mixes;
3) 2) in terpolymer EP rubber in add acvator, plasticating then mixes;
4) 3) in terpolymer EP rubber in add fire retardant, plasticating then mixes;
5) 4) in terpolymer EP rubber in add the filler of anti-the ablation, plasticating then mixes;
6) 5) in terpolymer EP rubber in add promotor, plasticating then mixes;
7) 6) in terpolymer EP rubber in add vulcanizing agent and silane coupling agent, plasticating then mixes;
8) with 7) in the mixture that mixes of plasticating be prefabricated into the base material by mold shape;
9) with 8) in the base material at room temperature place and vulcanize the terpolymer EP rubber mixture of anti-ablation that obtains containing ladder-like poly-phenyl silsesquioxane after 16～24 hours; Curing temperature is 160～170 ℃, and the time is 45～60 minutes, and pressure is 10～15MPa.
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|---|---|---|---|
| CN201010606018A CN102120849B (en) | 2010-12-15 | 2010-12-15 | Ethylene-propylene-diene monomer (EPDM) ablation-resistant composition containing high-regularity trapezoid polyphenyl silsesquioxane and preparation method thereof |
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| CN201010606018A CN102120849B (en) | 2010-12-15 | 2010-12-15 | Ethylene-propylene-diene monomer (EPDM) ablation-resistant composition containing high-regularity trapezoid polyphenyl silsesquioxane and preparation method thereof |
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| CN102120849B true CN102120849B (en) | 2012-10-24 |
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| CN103724828A (en) * | 2013-12-13 | 2014-04-16 | 芜湖佳诚电子科技有限公司 | Automobile cooling system sealing piece material |
| CN103772829B (en) * | 2014-01-24 | 2016-01-20 | 河南恒发橡塑制品有限公司 | Automotive trim environmental protection flame retardant rubber item and production technique thereof |
| CN105778298B (en) * | 2014-12-26 | 2018-03-20 | 湖北航天化学技术研究所 | A kind of EPDM heat-insulating materials of silicones filling |
| CN105131438A (en) * | 2015-09-02 | 2015-12-09 | 中国化工集团曙光橡胶工业研究设计院有限公司 | High-thermal-insulation ablation-resistant sizing material |
| CN105199245A (en) * | 2015-10-12 | 2015-12-30 | 苏州宽温电子科技有限公司 | Anti-aging insulating rubber material and preparation method thereof |
| CN106751005B (en) * | 2016-01-21 | 2020-05-05 | 湖北航天化学技术研究所 | Ethylene propylene diene monomer elastic heat-insulating material capable of resisting high overload ablation |
| CN106751015A (en) * | 2016-11-29 | 2017-05-31 | 湖北航天化学技术研究所 | A kind of EPDM of resistance to ablation heat-insulating materials of magnesium-based ceramics precursor filling |
| CN107434889A (en) * | 2017-09-20 | 2017-12-05 | 西安近代化学研究所 | A kind of low cigarette EPDM clad |
| CN109135073B (en) * | 2018-08-30 | 2020-06-02 | 北京理工大学 | Ablation-resistant ethylene propylene diene monomer composite material and preparation method thereof |
| CN108929494B (en) * | 2018-08-31 | 2020-09-11 | 北京理工大学 | Ethylene propylene diene monomer rubber for thermal protection of lithium ion battery and preparation method thereof |
| CN113480273B (en) * | 2021-08-17 | 2022-07-29 | 浙江省建设工程质量检验站有限公司 | Composite flame-retardant building material and preparation method thereof |
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| US20030212228A1 (en) * | 2002-05-02 | 2003-11-13 | Dso National Laboratories | Ladder-like silicone polymers |
| CN101735521A (en) * | 2009-12-18 | 2010-06-16 | 常熟市三恒建材有限责任公司 | Flame-retardant ethylene-propylene-diene waterproof sheet and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030212228A1 (en) * | 2002-05-02 | 2003-11-13 | Dso National Laboratories | Ladder-like silicone polymers |
| CN101735521A (en) * | 2009-12-18 | 2010-06-16 | 常熟市三恒建材有限责任公司 | Flame-retardant ethylene-propylene-diene waterproof sheet and preparation method thereof |
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Effective date of registration: 20140728 Address after: 100083, room 4, building 2, peony building, No. 412 peony, Haidian District, Beijing, Huayuan Road Patentee after: SUN-LIT WATERPROOF INSULATION ENGINEERING Co.,Ltd. Address before: 100081 No. 5, Zhongguancun South Street, Haidian District, Beijing Patentee before: BEIJING INSTITUTE OF TECHNOLOGY |
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Address after: 100083, room 4, building 2, peony building, No. 412 peony, Haidian District, Beijing, Huayuan Road Patentee after: Sanli Energy Conservation and Environmental Protection Engineering Co.,Ltd. Address before: 100083, room 4, building 2, peony building, No. 412 peony, Haidian District, Beijing, Huayuan Road Patentee before: SUN-LIT WATERPROOF INSULATION ENGINEERING Co.,Ltd. |
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Addressee: Wang Yanxia Document name: Notification of Passing Examination on Formalities |
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| DD01 | Delivery of document by public notice |