CN109370117B - 一种高阻燃耐老化氟橡胶电缆护套材料 - Google Patents
一种高阻燃耐老化氟橡胶电缆护套材料 Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 81
- 239000000463 material Substances 0.000 title claims abstract description 65
- 229920001973 fluoroelastomer Polymers 0.000 title claims abstract description 39
- 230000032683 aging Effects 0.000 title claims abstract description 36
- 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 claims abstract description 58
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 43
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 34
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 28
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 23
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- 230000003712 anti-aging effect Effects 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 17
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- OHRVBDRGLIWLPA-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] dihydrogen phosphate Chemical compound OCC(CO)(CO)COP(O)(O)=O OHRVBDRGLIWLPA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 241001122767 Theaceae Species 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
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- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 15
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- 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 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 14
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- 229910052624 sepiolite Inorganic materials 0.000 claims abstract description 12
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- 239000000203 mixture Substances 0.000 claims abstract description 11
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- 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 claims abstract description 10
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- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims abstract description 9
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 8
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- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 13
- 239000002956 ash Substances 0.000 claims description 13
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- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
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- -1 polyphenol hydroxyl acrylate Chemical class 0.000 claims description 7
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000006477 desulfuration reaction Methods 0.000 claims description 5
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- 239000003963 antioxidant agent Substances 0.000 claims 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
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- 229910052684 Cerium Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
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- 125000004432 carbon atom Chemical group C* 0.000 description 1
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- RMBPEFMHABBEKP-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2C3=C[CH]C=CC3=CC2=C1 RMBPEFMHABBEKP-UHFFFAOYSA-N 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
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- NIHNNTQXNPWCJQ-UHFFFAOYSA-N o-biphenylenemethane Natural products C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 1
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- LFGREXWGYUGZLY-UHFFFAOYSA-N phosphoryl Chemical group [P]=O LFGREXWGYUGZLY-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种高阻燃耐老化氟橡胶电缆护套材料,其原料包括:氟橡胶、丙烯酸酯橡胶、三元乙丙橡胶、硬脂酸、氧化镁、过氧化二异丙苯、三烯丙基三聚异氰酸酯、双酚AF、苄基三苯基氯化磷、氧化铈、白炭黑、纤维状海泡石、碱式硫酸镁晶须、硫酸锌、脱硫灰、硫酸钡、氧化铁、复合阻燃剂、防老剂;所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物。本发明提出的高阻燃耐老化氟橡胶电缆护套材料,其阻燃性能优异,耐热性和耐老化性好,永久变形小。
Description
技术领域
本发明涉及电缆材料技术领域,尤其涉及一种高阻燃耐老化氟橡胶电缆护套材料。
背景技术
氟橡胶是主链或侧链的碳原子接有氟原子的一类合成高分子弹性体,其具有良好的高温稳定性、耐介质能力、物理性能和电绝缘性,目前已被广泛用于现代航空、航天、火箭等尖端科学技术领域,但是氟橡胶也存在永久变形大和耐热性不是很好的缺陷,同时将其用于电缆中存在阻燃性、耐老化性和耐热性不足的缺陷,限制了其应用。
发明内容
基于背景技术存在的技术问题,本发明提出了一种高阻燃耐老化氟橡胶电缆护套材料,其阻燃性能优异,耐热性和耐老化性好,永久变形小。
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶80-90份、丙烯酸酯橡胶3-7份、三元乙丙橡胶7-13份、硬脂酸0.8-1.7份、氧化镁0.2-1.5份、过氧化二异丙苯2-3.5份、三烯丙基三聚异氰酸酯0.2-1.5份、双酚AF 0.3-1.5份、苄基三苯基氯化磷0.1-0.8份、氧化铈3-9份、白炭黑5-10份、纤维状海泡石2-11份、碱式硫酸镁晶须6-13份、硫酸锌3-6份、脱硫灰2-4份、硫酸钡1-5份、氧化铁1-3份、复合阻燃剂5-11份、防老剂0.5-2.8份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物。
优选地,所述丙烯酸酯橡胶为支化多酚羟基丙烯酸酯橡胶;具体以支化多酚羟基丙烯酸酯橡胶加入体系中,能利用支化多酚羟基丙烯酸酯橡胶中的酚羟基对基体起到硫化作用,提高了护套材料的拉伸强度、撕裂强度和断裂伸长率,同时改善了护套材料的压缩永久变形、耐老化性能、耐油性能和热稳定性。
优选地,所述碱式硫酸镁晶须为硅烷偶联剂KH-550改性碱式硫酸镁晶须;所述脱硫灰为硅烷偶联剂Si-69改性脱硫灰。
优选地,所述硫酸锌为改性硫酸锌;所述改性硫酸锌按照以下工艺进行制备:将丙酮和硫酸锌混合后球磨15-20h,加入丁腈橡胶后球磨2-5h,然后加入叔丁基对苯二酚,球磨5-10h,干燥得到所述改性硫酸锌。
优选地,硫酸锌、丁腈橡胶、叔丁基对苯二酚的重量比为10-25:50-80:20-35。
优选地,所述防老剂为防老剂D、防老剂4010NA中的一种或者两种的混合物。
优选地,复合阻燃剂中,笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的重量比为1-4:2-5:3-11:3-11:5-18。
优选地,所述磷氮阻燃剂按照以下工艺进行制备:将螺环磷酰二氯和4,4′-(9-芴)二苯酚加入乙腈中混合均匀,然后加入三乙醇胺,在密闭条件下进行超声反应2-3.5h,洗涤、干燥得到物料A;将物料A和咪唑加入二氯甲烷中,在55-65℃下搅拌反应2-5h,反应结束后冷却、过滤、干燥得到所述磷氮阻燃剂。
优选地,螺环磷酰二氯、4,4′-(9-芴)二苯酚的摩尔比为3-4:1;物料A、咪唑的摩尔比为1:2.2-3。
优选地,超声反应的温度为40-48℃,功率为120-150W。
本发明所述高阻燃耐老化氟橡胶电缆护套材料可以按照常规的氟橡胶复合材料制备工艺制备而成。
本发明所述高阻燃耐老化氟橡胶电缆护套材料,其以氟橡胶为主料,并加入了丙烯酸酯橡胶和三元乙丙橡胶配合,并控制了三者的含量,使三者相容性好,性能协同促进,同时选择了过氧化二异丙苯、三烯丙基三聚异氰酸酯、双酚AF、苄基三苯基氯化磷配合,实现了体系的共硫化,赋予护套材料优异的耐热性、耐油性、耐低温性和压缩永久变形性,同时改善了电缆护套材料的加工性能,克服了单纯的氟橡胶耐低温性和压缩永久变形性差的缺陷;氧化铈加入体系中,在纤维状海泡石和碱式硫酸镁晶须促进作用下,在基体中分散均匀,其表面的Si-OH以及Bronsted-Lewis酸中心具有高的化学活性,能使体系中的过氧化二异丙苯分解出更多的自由基,提高了护套材料的硫化速度,缩短了硫化的时间,提高了硫化效率,同时提高了护套材料的拉伸强度和扯断伸长率,同时铈元素能与硫化过程中产生的低分子物质形成配合物,进一步对护套材料起到了补强作用,其中,纤维状海泡石和碱式硫酸镁晶须具有良好的承载性,在护套材料压缩的过程中能承载部分压力用力,提高了护套材料的压缩永久变形性;硫酸锌的制备过程中,以硫酸锌、丁腈橡胶和叔丁基对苯二酚为原料,通过球磨的方式,使各原料的粒径更小,产生较多的交联点,使硫酸锌中的部分锌离子与丁腈橡胶中的氰基以及叔丁基对苯二酚中的酚羟基发生了配位反应,从而将锌离子、叔丁基对苯二酚、丁腈橡胶进行了交联,形成了更加密集的交联网络,加入体系中,与体系的相容性好,使分子链更不易被破坏,一方面抑制了大量的未配位的硫酸锌对分子链热氧分解的促进作用,与防老剂具有协同作用,提高了护套材料的耐老化性,同时一部分硫酸锌继续充当填料的作用,与白炭黑、纤维状海泡石、碱式硫酸镁晶须、脱硫灰、硫酸钡和氧化铁配合,起到了物理增强的作用,提高了护套材料的强度,同时赋予护套材料优异的耐热氧老化性能;复合阻燃剂具体选择了笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂进行配合,与纤维状海泡石和碱式硫酸镁晶须具有协同促进作用,提高了护套材料的氧指数,减小了热释放速率和生烟速率,赋予护套材料优异的阻燃性能,磷氮阻燃剂的制备过程中,首先以螺环磷酰二氯和4,4′-(9-芴)二苯酚为原料,控制反应的条件,使螺环磷酰二氯中的一个氯原子与4,4′-(9-芴)二苯酚中的酚羟基发生了反应,从而将螺环磷酰二氯和4,4′-(9-芴)二苯酚结合为一体,得到了物料A,物料A和咪唑混合后,咪唑中的氮原子能与物料A中的氯发生反应,从而将咪唑引入到了物料A中,得到了同时含有磷、氮和芴的磷氮阻燃剂,将其加体系中,在体系中分散均匀,与笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素配合,与纤维状海泡石和碱式硫酸镁晶须具有协同促进作用,在护套材料燃烧的过程中,在材料的表面形成了松散的“蠕虫状”结构,阻碍了热量和氧气向材料内部传递,同时磷氮阻燃剂、笼状季戊四醇磷酸酯分解生成的化合物填充了蠕虫状结构之间的孔洞,同时促进了橡胶基体的炭化,形成了坚固的炭层,起到了隔热隔氧的作用,减缓了火焰的蔓延,提高了护套材料的氧指数,减小了热释放速率和生烟速率,赋予护套材料优异的阻燃性能,同时将芴结构引入到了基体中,进一步提高了护套材料的耐热性。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶90份、丙烯酸酯橡胶3份、三元乙丙橡胶13份、硬脂酸0.8份、氧化镁1.5份、过氧化二异丙苯2份、三烯丙基三聚异氰酸酯1.5份、双酚AF 0.3份、苄基三苯基氯化磷0.8份、氧化铈3份、白炭黑10份、纤维状海泡石2份、碱式硫酸镁晶须13份、硫酸锌3份、脱硫灰4份、硫酸钡1份、氧化铁3份、复合阻燃剂5份、防老剂2.8份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物。
对本实施例的高阻燃耐老化氟橡胶电缆护套材料进行性能检测,其极限氧指数为41;拉伸强度为19.4MPa,断裂伸长率为753%,邵尔A硬度为87,扯断永久变形为1.5%;在275℃下老化24h后,拉伸强度变化率为-5.8%,断裂伸长率变化率为-5.9%,硬度变化为+4。
实施例2
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶80份、丙烯酸酯橡胶7份、三元乙丙橡胶7份、硬脂酸1.7份、氧化镁0.2份、过氧化二异丙苯3.5份、三烯丙基三聚异氰酸酯0.2份、双酚AF 1.5份、苄基三苯基氯化磷0.1份、氧化铈9份、白炭黑5份、纤维状海泡石11份、碱式硫酸镁晶须6份、硫酸锌6份、脱硫灰2份、硫酸钡5份、氧化铁1份、复合阻燃剂11份、防老剂0.5份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物。
对本实施例的高阻燃耐老化氟橡胶电缆护套材料进行性能检测,其极限氧指数为43;拉伸强度为18.7MPa,断裂伸长率为653%,邵尔A硬度为76,扯断永久变形为2.8%;在275℃下老化24h后,拉伸强度变化率为-7.8%,断裂伸长率变化率为-6.5%,硬度变化为+6。
实施例3
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶88份、丙烯酸酯橡胶4份、三元乙丙橡胶11份、硬脂酸0.9份、氧化镁1.3份、过氧化二异丙苯2.6份、三烯丙基三聚异氰酸酯1.3份、双酚AF 0.6份、苄基三苯基氯化磷0.7份、氧化铈4份、白炭黑9.3份、纤维状海泡石4.5份、碱式硫酸镁晶须12份、硫酸锌3.8份、脱硫灰3.8份、硫酸钡2份、氧化铁2.7份、复合阻燃剂7份、防老剂2.5份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物;
所述丙烯酸酯橡胶为支化多酚羟基丙烯酸酯橡胶;
所述碱式硫酸镁晶须为硅烷偶联剂KH-550改性碱式硫酸镁晶须;所述脱硫灰为硅烷偶联剂Si-69改性脱硫灰;
所述硫酸锌为改性硫酸锌;所述改性硫酸锌按照以下工艺进行制备:将丙酮和硫酸锌混合后球磨15h,加入丁腈橡胶后球磨5h,然后加入叔丁基对苯二酚,球磨5h,干燥得到所述改性硫酸锌;其中,硫酸锌、丁腈橡胶、叔丁基对苯二酚的重量比为25:50:35;
所述防老剂为防老剂D;
复合阻燃剂中,笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的重量比为1:5:3:11:5;
所述磷氮阻燃剂按照以下工艺进行制备:将螺环磷酰二氯和4,4′-(9-芴)二苯酚加入乙腈中混合均匀,然后加入三乙醇胺,在密闭条件下进行超声反应2h,洗涤、干燥得到物料A;将物料A和咪唑加入二氯甲烷中,在65℃下搅拌反应2h,反应结束后冷却、过滤、干燥得到所述磷氮阻燃剂,其中,螺环磷酰二氯、4,4′-(9-芴)二苯酚的摩尔比为4:1;物料A、咪唑的摩尔比为1:2.2;超声反应的温度为48℃,功率为120W。
对本实施例的高阻燃耐老化氟橡胶电缆护套材料进行性能检测,其极限氧指数为48;拉伸强度为21.8MPa,断裂伸长率为553%,邵尔A硬度为69,扯断永久变形为3.1%;在275℃下老化24h后,拉伸强度变化率为-6.1%,断裂伸长率变化率为-5.1%,硬度变化为+3。
实施例4
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶83份、丙烯酸酯橡胶6份、三元乙丙橡胶8份、硬脂酸1.5份、氧化镁0.5份、过氧化二异丙苯3.2份、三烯丙基三聚异氰酸酯0.5份、双酚AF 1.4份、苄基三苯基氯化磷0.3份、氧化铈8.3份、白炭黑6.2份、纤维状海泡石9份、碱式硫酸镁晶须8份、硫酸锌5.8份、脱硫灰2.6份、硫酸钡4.7份、氧化铁1.3份、复合阻燃剂10份、防老剂0.9份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物;
所述丙烯酸酯橡胶为支化多酚羟基丙烯酸酯橡胶;
所述碱式硫酸镁晶须为硅烷偶联剂KH-550改性碱式硫酸镁晶须;所述脱硫灰为硅烷偶联剂Si-69改性脱硫灰;
所述硫酸锌为改性硫酸锌;所述改性硫酸锌按照以下工艺进行制备:将丙酮和硫酸锌混合后球磨20h,加入丁腈橡胶后球磨2h,然后加入叔丁基对苯二酚,球磨10h,干燥得到所述改性硫酸锌;其中,硫酸锌、丁腈橡胶、叔丁基对苯二酚的重量比为10:80:20;
所述防老剂为防老剂4010NA;
复合阻燃剂中,笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的重量比为4:2:11:3:18;
所述磷氮阻燃剂按照以下工艺进行制备:将螺环磷酰二氯和4,4′-(9-芴)二苯酚加入乙腈中混合均匀,然后加入三乙醇胺,在密闭条件下进行超声反应3.5h,洗涤、干燥得到物料A;将物料A和咪唑加入二氯甲烷中,在55℃下搅拌反应5h,反应结束后冷却、过滤、干燥得到所述磷氮阻燃剂,其中,螺环磷酰二氯、4,4′-(9-芴)二苯酚的摩尔比为3:1;物料A、咪唑的摩尔比为1:3;超声反应的温度为40℃,功率为150W。
对本实施例的高阻燃耐老化氟橡胶电缆护套材料进行性能检测,其极限氧指数为46;拉伸强度为19.8MPa,断裂伸长率为557%,邵尔A硬度为63,扯断永久变形为3.2%;在275℃下老化24h后,拉伸强度变化率为-5.9%,断裂伸长率变化率为-5.3%,硬度变化为+5。
实施例5
本发明提出的一种高阻燃耐老化氟橡胶电缆护套材料,其原料按重量份包括:氟橡胶85份、丙烯酸酯橡胶5.5份、三元乙丙橡胶12份、硬脂酸1.3份、氧化镁1份、过氧化二异丙苯2.8份、三烯丙基三聚异氰酸酯1.2份、双酚AF 1份、苄基三苯基氯化磷0.5份、氧化铈6份、白炭黑8份、纤维状海泡石7份、碱式硫酸镁晶须9份、硫酸锌5.7份、脱硫灰3.8份、硫酸钡2.8份、氧化铁2份、复合阻燃剂8份、防老剂2.3份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物;
所述丙烯酸酯橡胶为支化多酚羟基丙烯酸酯橡胶;
所述碱式硫酸镁晶须为硅烷偶联剂KH-550改性碱式硫酸镁晶须;所述脱硫灰为硅烷偶联剂Si-69改性脱硫灰;
所述硫酸锌为改性硫酸锌;所述改性硫酸锌按照以下工艺进行制备:将丙酮和硫酸锌混合后球磨17h,加入丁腈橡胶后球磨3.8h,然后加入叔丁基对苯二酚,球磨8h,干燥得到所述改性硫酸锌;其中,硫酸锌、丁腈橡胶、叔丁基对苯二酚的重量比为16:63:28;
所述防老剂为防老剂D、防老剂4010NA的混合物,且防老剂D、防老剂4010NA的重量比为3:5;
复合阻燃剂中,笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的重量比为3:4:7:8:12;
所述磷氮阻燃剂按照以下工艺进行制备:将螺环磷酰二氯和4,4′-(9-芴)二苯酚加入乙腈中混合均匀,然后加入三乙醇胺,在密闭条件下进行超声反应2.8h,洗涤、干燥得到物料A;将物料A和咪唑加入二氯甲烷中,在60℃下搅拌反应3.5h,反应结束后冷却、过滤、干燥得到所述磷氮阻燃剂,其中,螺环磷酰二氯、4,4′-(9-芴)二苯酚的摩尔比为3.8:1;物料A、咪唑的摩尔比为1:2.7;超声反应的温度为45℃,功率为138W。
对本实施例的高阻燃耐老化氟橡胶电缆护套材料进行性能检测,其极限氧指数为49;拉伸强度为23.8MPa,断裂伸长率为775%,邵尔A硬度为73,扯断永久变形为2.1%;在275℃下老化24h后,拉伸强度变化率为-2.9%,断裂伸长率变化率为-2.7%,硬度变化为+2。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种高阻燃耐老化氟橡胶电缆护套材料,其特征在于,其原料按重量份包括:氟橡胶80-90份、丙烯酸酯橡胶3-7份、三元乙丙橡胶7-13份、硬脂酸0.8-1.7份、氧化镁0.2-1.5份、过氧化二异丙苯2-3.5份、三烯丙基三聚异氰酸酯0.2-1.5份、双酚AF 0.3-1.5份、苄基三苯基氯化磷0.1-0.8份、氧化铈3-9份、白炭黑5-10份、纤维状海泡石2-11份、碱式硫酸镁晶须6-13份、硫酸锌3-6份、脱硫灰2-4份、硫酸钡1-5份、氧化铁1-3份、复合阻燃剂5-11份、防老剂0.5-2.8份;
其中,所述复合阻燃剂为笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的混合物;
其中,所述硫酸锌为改性硫酸锌;所述改性硫酸锌按照以下工艺进行制备:将丙酮和硫酸锌混合后球磨15-20h,加入丁腈橡胶后球磨2-5h,然后加入叔丁基对苯二酚,球磨5-10h,干燥得到所述改性硫酸锌;
其中,所述丙烯酸酯橡胶为支化多酚羟基丙烯酸酯橡胶;
其中,所述磷氮阻燃剂按照以下工艺进行制备:将螺环磷酰二氯和4,4′-(9-芴)二苯酚加入乙腈中混合均匀,然后加入三乙醇胺,在密闭条件下进行超声反应2-3.5h,洗涤、干燥得到物料A;将物料A和咪唑加入二氯甲烷中,在55-65℃下搅拌反应2-5h,反应结束后冷却、过滤、干燥得到所述磷氮阻燃剂。
2.根据权利要求1所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,所述碱式硫酸镁晶须为硅烷偶联剂KH-550改性碱式硫酸镁晶须;所述脱硫灰为硅烷偶联剂Si-69改性脱硫灰。
3.根据权利要求1所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,硫酸锌、丁腈橡胶、叔丁基对苯二酚的重量比为10-25:50-80:20-35。
4.根据权利要求1或2所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,所述防老剂为防老剂D、防老剂4010NA中的一种或者两种的混合物。
5.根据权利要求1或2所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,复合阻燃剂中,笼状季戊四醇磷酸酯、可膨胀石墨、硼酸锌、茶皂素、磷氮阻燃剂的重量比为1-4:2-5:3-11:3-11:5-18。
6.根据权利要求1所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,螺环磷酰二氯、4,4′-(9-芴)二苯酚的摩尔比为3-4:1;物料A、咪唑的摩尔比为1:2.2-3。
7.根据权利要求1或6所述高阻燃耐老化氟橡胶电缆护套材料,其特征在于,超声反应的温度为40-48℃,功率为120-150W。
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