CN115418046B - 耐泥耐腐蚀船舶用电缆料 - Google Patents
耐泥耐腐蚀船舶用电缆料 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000005260 corrosion Methods 0.000 title claims abstract description 34
- 230000007797 corrosion Effects 0.000 title claims abstract description 34
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 55
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 52
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 27
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 25
- 239000011737 fluorine Substances 0.000 claims abstract description 25
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
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- 239000000314 lubricant Substances 0.000 claims abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 82
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 53
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 24
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 229910021389 graphene Inorganic materials 0.000 claims description 21
- HKILWKSIMZSWQX-UHFFFAOYSA-N tris(prop-2-enyl)silane Chemical compound C=CC[SiH](CC=C)CC=C HKILWKSIMZSWQX-UHFFFAOYSA-N 0.000 claims description 21
- 239000007818 Grignard reagent Substances 0.000 claims description 18
- -1 allyl bromide Grignard reagent Chemical class 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- BHELZAPQIKSEDF-UHFFFAOYSA-N allyl bromide Chemical compound BrCC=C BHELZAPQIKSEDF-UHFFFAOYSA-N 0.000 claims description 14
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 13
- 239000005052 trichlorosilane Substances 0.000 claims description 13
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 12
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
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- 229920001903 high density polyethylene Polymers 0.000 claims description 5
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- 239000002904 solvent Substances 0.000 claims description 5
- WEUBQNJHVBMUMD-UHFFFAOYSA-N trichloro(3,3,3-trifluoropropyl)silane Chemical compound FC(F)(F)CC[Si](Cl)(Cl)Cl WEUBQNJHVBMUMD-UHFFFAOYSA-N 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
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- 238000001816 cooling Methods 0.000 claims description 3
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- 239000011159 matrix material Substances 0.000 abstract description 15
- 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 description 13
- 239000003063 flame retardant Substances 0.000 abstract description 13
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- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 4
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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 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
- 239000008116 calcium stearate Substances 0.000 description 2
- 235000013539 calcium stearate Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
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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 description 1
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- RBQXWIGHVHFTKW-UHFFFAOYSA-N dichloro-propyl-(trifluoromethyl)silane Chemical compound FC([Si](Cl)(Cl)CCC)(F)F RBQXWIGHVHFTKW-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
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- 230000008569 process Effects 0.000 description 1
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- 239000012085 test solution Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2203/00—Applications
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
本发明涉及耐泥耐腐蚀船舶用电缆料,属于电缆料制备技术领域,包括以下重量份原料:基础树脂85‑100份、炭黑8‑10份、改性聚磷酸铵25‑30份、改性氧化石墨烯5‑8份、偶联剂0.7‑1.2份、交联剂1‑2份、抗氧剂1.5‑2.5份和润滑剂0.8‑1.2份;将上述原料混合,挤出造粒即可,在基料中引入了改性聚磷酸铵和改性氧化石墨烯,两者在基体中分散性好,阻燃性能高、耐迁移、耐湿热,且基于氟硅的低表面能特点,将改性聚磷酸铵加入电缆料中,不仅能够提高电缆料的耐腐蚀性能,还能提高其阻燃性能,改性氧化石墨烯在基体中形成有机无机杂化网络,分散应力、吸收能量,提高电缆料整体的力学性能、耐腐蚀和阻燃性能。
Description
技术领域
本发明属于电缆料制备技术领域,具体地,涉及一种耐泥耐腐蚀船舶用电缆料。
背景技术
随着经济形势的变化,造船业由以前的粗放型开始向精细化方向发展,对配套设备和材料也提出更高的要求,尤其是船舶用电缆的综合性能,不仅要求具有良好的电性能,更重要的是应具备耐泥(泥浆钻井液)和耐腐蚀(燃油、润滑油、酸碱液)性能,现有的电缆护套材料在测试液中拉伸强度变化率和体积膨胀率均超过20%,如公开号为CN104927176B和CN103030874B的专利中所述的电缆料,可见耐泥耐腐蚀性能并不是很好,且上述专利为了使电缆料达到耐火标准添加了大量无机阻燃剂(氢氧化铝和氢氧化镁),虽然提高了阻燃性能,但是这些无机粒子在聚合物基质中由于极性差异较大难以分散均匀,造成电缆料力学性能降低,进而在受到外力作用时,造成电缆护套开裂破损等影响,进一步地削弱电缆料的耐腐蚀性能。
发明内容
为了解决背景技术中提到的技术问题,本发明提供一种耐泥耐腐蚀船舶用电缆料。
本发明的目的可以通过以下技术方案实现:
耐泥耐腐蚀船舶用电缆料,包括以下重量份原料:基础树脂85-100份、炭黑8-10份、改性聚磷酸铵25-30份、改性氧化石墨烯5-8份、偶联剂0.7-1.2份、交联剂1-2份、抗氧剂1.5-2.5份和润滑剂0.8-1.2份;
该耐泥耐腐蚀船舶用电缆料通过以下步骤制成:
将上述原料在高速混合机中混合20-30mi n,转移至双螺杆挤出机中挤出造粒,得到耐泥耐腐蚀船舶用电缆料,双螺杆挤出机温度为100-160℃。
进一步地,改性聚磷酸铵通过以下步骤制成:
步骤S11、按照乙醇和去离子水体积比1:4制备乙醇溶液,加入三甲氧基硅烷,利用乙酸调节pH为3.5-5.5,在50℃下水解反应1-2h后加入聚磷酸铵(APP),升温至60℃,搅拌反应1-2h,反应结束后,抽滤、干燥、粉碎,得到活化APP,乙醇溶液、三甲氧基硅烷和聚磷酸铵的用量比为5-8mL:0.5g:12.5g;
步骤S12、在氮气保护下,将活化APP、含氟三烯丙基硅烷、三氯硅烷、重蒸THF和铂催化剂依次加入三口烧瓶中,升温至60℃下搅拌反应5-6h,减压蒸馏去除THF和过量的三氯硅烷,得到中间产物,将中间产物溶于无水***中,0-5℃下滴加烯丙基溴格氏试剂溶液,滴加完毕后,室温下搅拌12-14h,后处理,得到改性聚磷酸铵,活化APP、含氟三烯丙基硅烷、三氯硅烷、重蒸THF、无水***和烯丙基溴格氏试剂溶液的用量比为10g:10mmol:40-50mmol:100-120mL:20mL:70-80mL,铂催化剂为氯铂酸,氯铂酸用量为含氟三烯丙基硅烷和三氯硅烷质量和的0.05-0.5%,后处理同含氟三烯丙基硅烷制备。
聚磷酸铵是一种无机高分子磷酸盐,与有机聚合物基体的相容性差,并且容易析出、吸湿、阻燃效率不高,因此利用三甲氧基硅烷对其进行初步活化,在其表面引入活性-Si-H增加活性位点,为后续反应奠定基础,然后以活化APP、含氟三烯丙基硅烷、三氯硅烷为反应原料,通过硅氢加成反应在APP表面引入含氟支化聚碳硅烷,最后利用烯丙基溴格氏试剂进行端基处理,得到端不饱和双键、含氟超支化聚碳硅烷接枝APP,即改性聚磷酸铵,含氟超支化聚碳硅烷的引入一方面提高APP表面的疏水性,克服其易吸湿和易迁移性的问题,另一方面利用超支化聚合物流动性高、溶解好和热稳定性高的特点,提高APP在基材的分散性,通过端部活性基团与聚合基质发生交联反应,使APP通过化学链锚固于基材内部,更好的发挥阻燃性能,更为突出的是,聚碳硅烷本身是一类有机硅高分子物质,其主链由硅和碳原子交替组成,具有耐高温、耐腐蚀和耐腐蚀特性,并且在高温下裂解产生SiC陶瓷相,在陶瓷化过程中增加APP颗粒之间的致密性,提高其阻燃效果,因此,将改性聚磷酸铵加入电缆料中,在不破坏基体机械性能的前提下,不仅能够提高电缆料的耐腐蚀性能,还能提高其阻燃性能。
进一步地,含氟三烯丙基硅烷由以下步骤制成:
在无水无氧条件,将三氟丙基三氯硅烷加入***中,搅拌后0-5℃下缓慢滴加至烯丙基溴格氏试剂溶液,滴加结束后,室温下搅拌反应12h后,后处理,具体为:将上清液转移至分液漏斗中,沉淀物则经布氏漏斗减压抽滤,用***洗涤3次后,合并滤液和上清液,滴加0-5℃的饱和氯化铵水溶液直至无气泡产生,有机相依次用饱和氯化钠水溶液洗涤3次,无水硫酸镁干燥后,60℃下旋蒸去除***,得到含氟三烯丙基硅烷;
其中,三氟丙基三氯硅烷、***和烯丙基溴格氏试剂溶液的用量比为23.4-24.5mmol:30-40mL:70mL,以三氟丙基甲基二氯硅烷与烯丙基溴格氏试剂反应,得到含氟三烯丙基硅烷,反应过程如下:
所述烯丙基溴格氏试剂溶液通过以下步骤制成:
在无水无氧条件下,将镁屑和碘置于三口烧瓶中,加入***,降温至0-5℃缓慢滴加烯丙基溴的***溶液,滴加结束后,0-5℃下反应2h,得到烯丙基溴格氏试剂溶液,镁屑、碘、***和烯丙基溴的***溶液的用量比为3g:0.2-0.25g:50mL:20mL,烯丙基溴的***溶液中烯丙基溴和***的用量比为105mmol:20mL。
进一步地,改性氧化石墨烯通过以下步骤制成:
步骤S21、将氧化石墨烯超声分散于乙醇溶液中,加入KH-590水解液,升温至60-70℃,搅拌反应4-5h,抽滤,滤饼用乙醇溶液洗涤3-5次,干燥,得到巯基化氧化石墨烯;
其中,乙醇溶液由无水乙醇和去离子水按照体积比1:4组成,氧化石墨烯、乙醇溶液和KH-590水解液用量比为3g:100mL:2.4-3.0mL,KH-590水解液通过将偶联剂KH-590加入其6-8倍体积的乙醇溶液中,并用乙酸调节pH为4-5,室温水解2h得到;
步骤S22、将安息香二甲醚加入四氢呋喃和甲醇按照体积比3:1组成的溶剂中,加入乙烯基POSS,搅拌均匀后加入巯基化氧化石墨烯,超声振荡5min后,在波长365nm、800W紫外灯下反应15-20min,反应结束后,旋蒸去除溶剂,得到改性氧化石墨烯;
其中,巯基化氧化石墨烯和乙烯基POSS的质量比为1:0.1-0.2,安息香二甲醚用量为巯基化氧化石墨烯和乙烯基POSS质量和的2%。
基于氧化石墨烯良好的阻隔效果和热稳定性,先利用KH-590对其进行巯基化处理,进而通过巯基-烯点击反应在表面接枝乙烯基POSS,利用乙烯基POSS多活性位点效应,提高氧化石墨烯在基体中的分散性同时赋予其交联反应能力,乙烯基POSS在高温下使聚合物表面形成炭层,与氧化石墨烯协同发挥隔热、隔氧作用,并且能够与聚合物基质或者改性聚磷酸铵发生接枝反应,在基体中形成有机无机杂化网络,提高基体整体的力学性能、耐腐蚀和阻燃性能。
其中,基础树脂由高密度聚乙烯和乙烯醋酸乙烯共聚物按照质量比20-30:70-80组成,炭黑粒径为12-30nm。
进一步地,偶联剂为硅烷偶联剂A-172或Z-6173。
进一步地,交联剂为三烯丙基异氰脲酸酯、三甲代烯丙基异氰酸酯、过氧化二异丙苯和双叔丁基过氧异丙基苯中的一种或多种按照任意比例组成。
进一步地,抗氧剂为抗氧剂1010和抗氧剂DLTP按照质量比0.8-1:1-1.2组成。
进一步地,润滑剂为PE蜡、EVA蜡、硬脂酸钙或硬脂酸锌中的至少一种。
本发明的有益效果:
发明提供一种耐泥耐腐蚀船舶用电缆料,在基料中引入了改性聚磷酸铵和改性氧化石墨烯,改性聚磷酸不仅在基体中分散性好,且阻燃性能高、耐迁移、耐湿热,且由于含氟聚碳硅烷的引入,基于氟硅的低表面能特点,将改性聚磷酸铵加入电缆料中,不仅能够提高电缆料的耐腐蚀性能,还能提高其阻燃性能,改性氧化石墨烯在基体中同样具有良好的分散性,并且由于乙烯基POSS的引入,氧化石墨烯被牢固锚定在基体中,在基体中与其他材料相互作用,形成“迷宫式”的物理屏障,隔离泥浆和燃油的侵蚀,且能够与聚合物基质或者改性聚磷酸铵发生接枝反应,在基体中形成有机无机杂化网络,分散应力、吸收能量,提高电缆料整体的力学性能、耐腐蚀和阻燃性能,综上,本发明制备的船舶用电缆料不仅具有优异的耐泥耐腐蚀性,还具有良好的力学性能和阻燃性能。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
改性聚磷酸铵的制备:
步骤S11、按照乙醇和去离子水体积比1:4制备5mL乙醇溶液,加入0.5g三甲氧基硅烷,利用乙酸调节pH为3.5,在50℃下水解反应1h后加入12.5g聚磷酸铵,升温至60℃,搅拌反应1h,抽滤、干燥、粉碎,得到活化APP;
步骤S12、在无水无氧条件下,将3g镁屑和0.2g碘置于三口烧瓶中,加入50mL***,降温至0℃缓慢滴加烯丙基溴的***溶液,滴加结束后,0℃下反应2h,得到烯丙基溴格氏试剂溶液,烯丙基溴的***溶液中烯丙基溴和***的用量比为105mmol:20mL;
步骤S13、在氮气保护下,将10g活化APP、10mmol含氟三烯丙基硅烷、40mmol三氯硅烷、100mL重蒸THF和铂催化剂依次加入三口烧瓶中,升温至60℃下搅拌反应5h,减压蒸馏去除THF和过量的三氯硅烷,得到中间产物,将中间产物溶于20mL无水***中,0℃下滴加70mL烯丙基溴格氏试剂溶液,室温下搅拌12h,后处理,得到改性聚磷酸铵,铂催化剂为氯铂酸,氯铂酸用量为含氟三烯丙基硅烷和三氯硅烷质量和的0.05%,后处理同含氟三烯丙基硅烷制备。
所述含氟三烯丙基硅烷由以下步骤制成:
在无水无氧条件,将23.4mmol三氟丙基三氯硅烷加入30mL***中,搅拌后0℃下缓慢滴加至70mL烯丙基溴格氏试剂溶液,滴加结束后,室温下搅拌反应12h后,后处理,具体为:将上清液转移至分液漏斗中,沉淀物则经布氏漏斗减压抽滤,用***洗涤3次后,合并滤液和上清液,滴加0℃的饱和氯化铵水溶液直至无气泡产生,有机相依次用饱和氯化钠水溶液洗涤3次,无水硫酸镁干燥后,60℃下旋蒸去除***,得到含氟三烯丙基硅烷。
实施例2
改性聚磷酸铵的制备:
步骤S11、按照乙醇和去离子水体积比1:4制备8mL乙醇溶液,加入0.5g三甲氧基硅烷,利用乙酸调节pH为5.5,在50℃下水解反应2h后加入12.5g聚磷酸铵,升温至60℃,搅拌反应2h,反应结束后,抽滤、干燥、粉碎,得到活化APP;
步骤S12、在无水无氧条件下,将3g镁屑和0.25g碘置于三口烧瓶中,加入50mL***,降温至5℃缓慢滴加烯丙基溴的***溶液,5℃下反应2h,得到烯丙基溴格氏试剂溶液,烯丙基溴的***溶液中烯丙基溴和***的用量比为105mmol:20mL;
步骤S13、在氮气保护下,将10g活化APP、10mmol含氟三烯丙基硅烷、50mmol三氯硅烷、120mL重蒸THF和铂催化剂依次加入三口烧瓶中,升温至60℃下搅拌反应6h,减压蒸馏去除THF和过量的三氯硅烷,得到中间产物,将中间产物溶于20mL无水***中,5℃下滴加80mL烯丙基溴格氏试剂溶液,滴加完毕后,室温下搅拌14h,后处理,得到改性聚磷酸铵,铂催化剂为氯铂酸,氯铂酸用量为含氟三烯丙基硅烷和三氯硅烷质量和的0.5%,后处理同含氟三烯丙基硅烷制备。
含氟三烯丙基硅烷同实施例1。
对比例1
按照乙醇和去离子水体积比1:4制备8mL乙醇溶液,加入0.5g硅烷偶联剂KH-570,利用乙酸调节pH为5.5,在50℃下水解反应2h后加入12.5g聚磷酸铵,升温至60℃,搅拌反应2h,反应结束后,抽滤、干燥、粉碎,得到改性聚磷酸铵。
实施例3
改性氧化石墨烯的制备:
步骤S21、将3g氧化石墨烯超声分散于100mL乙醇溶液中,加入2.4mL KH-590水解液,升温至60℃,搅拌反应4h,抽滤,滤饼用乙醇溶液洗涤3次,干燥,得到巯基化氧化石墨烯,乙醇溶液由无水乙醇和去离子水按照体积比1:4组成,KH-590水解液通过将偶联剂KH-590加入其6倍体积的乙醇溶液中,并用乙酸调节pH为4,室温水解2h得到;
步骤S22、将1g安息香二甲醚加入10mL四氢呋喃和甲醇按照体积比3:1组成的溶剂中,加入0.1g乙烯基POSS,搅拌均匀后加入巯基化氧化石墨烯,超声振荡5min后,在波长365nm、800W紫外灯下反应15min,反应结束后,旋蒸去除溶剂,得到改性氧化石墨烯,安息香二甲醚用量为巯基化氧化石墨烯和乙烯基POSS质量和的2%。
实施例4
改性氧化石墨烯的制备:
步骤S21、将3g氧化石墨烯超声分散于100mL乙醇溶液中,加入3.0mL KH-590水解液,升温至70℃,搅拌反应5h,抽滤,滤饼用乙醇溶液洗涤5次,干燥,得到巯基化氧化石墨烯,乙醇溶液由无水乙醇和去离子水按照体积比1:4组成,KH-590水解液通过将偶联剂KH-590加入其8倍体积的乙醇溶液中,并用乙酸调节pH为5,室温水解2h得到;
步骤S22、将1g安息香二甲醚加入20mL四氢呋喃和甲醇按照体积比3:1组成的溶剂中,加入0.2g乙烯基POSS,搅拌均匀后加入巯基化氧化石墨烯,超声振荡5min后,在波长365nm、800W紫外灯下反应20min,反应结束后,旋蒸去除溶剂,得到改性氧化石墨烯,安息香二甲醚用量为巯基化氧化石墨烯和乙烯基POSS质量和的2%。
对比例2
本对比例为实施例3步骤S21所得物质。
实施例5
耐泥耐腐蚀船舶用电缆料,包括以下重量份原料:基础树脂85份、炭黑8份、实施例1改性聚磷酸铵25份、实施例3改性氧化石墨烯5份、硅烷偶联剂A-172 0.7份、三甲代烯丙基异氰酸酯1份、抗氧剂1.5份和PE蜡0.8份;
通过以下步骤制成:
将上述原料在高速混合机中混合20min,转移至双螺杆挤出机中挤出造粒,得到耐泥耐腐蚀船舶用电缆料,双螺杆挤出机温度为100-160℃。
基础树脂由高密度聚乙烯(熔体指数0.08g/10min)和乙烯醋酸乙烯共聚物按(熔体指数0.2g/10min)照质量比2:8组成,炭黑粒径为12-30nm,抗氧剂为抗氧剂1010和抗氧剂DLTP按照质量比0.8:1组成。
实施例6
耐泥耐腐蚀船舶用电缆料,包括以下重量份原料:基础树脂90份、炭黑8份、实施例1改性聚磷酸铵28份、实施例4改性氧化石墨烯7份、硅烷偶联剂A-172 0.9份、三烯丙基异氰脲酸酯1.5份、抗氧剂2.0份和EVA蜡1.0份;
通过以下步骤制成:
将上述原料在高速混合机中混合25min,转移至双螺杆挤出机中挤出造粒,得到耐泥耐腐蚀船舶用电缆料,双螺杆挤出机温度为100-160℃。
基础树脂由高密度聚乙烯(熔体指数0.08g/10min)和乙烯醋酸乙烯共聚物按(熔体指数0.2g/10min)照质量比3:7组成,炭黑粒径为12-30nm,抗氧剂为抗氧剂1010和抗氧剂DLTP按照质量比1:1.2组成。
实施例7
耐泥耐腐蚀船舶用电缆料,包括以下重量份原料:基础树脂100份、炭黑10份、实施例2改性聚磷酸铵30份、实施例3改性氧化石墨烯8份、硅烷偶联剂A-172 1.2份、三甲代烯丙基异氰酸酯2份、抗氧剂2.5份和硬脂酸钙1.2份;
通过以下步骤制成:
将上述原料在高速混合机中混合30min,转移至双螺杆挤出机中挤出造粒,得到耐泥耐腐蚀船舶用电缆料,双螺杆挤出机温度为100-160℃。
基础树脂由高密度聚乙烯(熔体指数0.08g/10min)和乙烯醋酸乙烯共聚物按(熔体指数0.2g/10min)照质量比3:8组成,炭黑粒径为12-30nm,抗氧剂为抗氧剂1010和抗氧剂DLTP按照质量比1:1.2组成。
对比例3
将实施例5中改性聚磷酸铵替换成对比例1中物质,其余原料及制备过程同实施例5。
对比例4
将实施例6中改性氧化石墨烯替换成对比例2中物质,其余原料及制备过程同实施例6。
对实施例5-7和对比例3-4所制备的电缆料进行测试,参考标准IEC60092-359测试拉伸强度,ISO 4589测试氧指数,NEK606:2009测试耐油和耐泥浆性能,测试结果如表1所示:
表1
由表1可以看出,相比于对比例3-4,实施例5-7所制备的电缆料不仅具有良好的耐腐蚀耐泥浆性能,且力学性能好,阻燃性能高。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (7)
1.耐泥耐腐蚀船舶用电缆料,其特征在于,包括以下重量份原料:基础树脂85-100份、炭黑8-10份、改性聚磷酸铵25-30份、改性氧化石墨烯5-8份、偶联剂0.7-1.2份、交联剂1-2份、抗氧剂1.5-2.5份和润滑剂0.8-1.2份;
所述改性聚磷酸铵通过以下步骤制成:
在氮气保护下,将活化APP、含氟三烯丙基硅烷、三氯硅烷、重蒸THF和铂催化剂混合,60℃下搅拌反应5-6h,减压蒸馏得到中间产物,将中间产物溶于无水***中,0-5℃下滴加烯丙基溴格氏试剂溶液,滴加完毕后,室温下搅拌12-14h,后处理,得到改性聚磷酸铵;
活化APP通过以下步骤制成:
按照乙醇和去离子水体积比1:4制备乙醇溶液,加入三甲氧基硅烷,利用乙酸调节pH为3.5-5.5,在50℃下水解反应1-2h后加入聚磷酸铵,升温至60℃,搅拌反应1-2h,得到活化APP;
含氟三烯丙基硅烷由以下步骤制成:
在无水无氧条件,将三氟丙基三氯硅烷加入***中,搅拌后0-5℃下缓慢滴加至烯丙基溴格氏试剂溶液,滴加结束后,室温下搅拌反应12h后,后处理,得到含氟三烯丙基硅烷;
改性氧化石墨烯通过以下步骤制成:
步骤S21、将氧化石墨烯超声分散于乙醇溶液中,加入KH-590水解液,升温至60-70℃,搅拌反应4-5h,得到巯基化氧化石墨烯;
步骤S22、将安息香二甲醚加入四氢呋喃和甲醇按照体积比3:1组成的溶剂中,加入乙烯基POSS,搅拌后加入巯基化氧化石墨烯,超声振荡后,在波长365nm、800W紫外灯下反应15-20min,得到改性氧化石墨烯;
基础树脂由高密度聚乙烯和乙烯醋酸乙烯共聚物按照质量比20-30:70-80组成。
2.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,铂催化剂为氯铂酸,氯铂酸用量为含氟三烯丙基硅烷和三氯硅烷质量和的0.05-0.5%。
3.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,乙醇溶液、三甲氧基硅烷和聚磷酸铵的用量比为5-8mL:0.5g:12.5g。
4.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,三氟丙基三氯硅烷、***和烯丙基溴格氏试剂溶液的用量比为23.4-24.5mmol:30-40mL:70mL。
5.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,所述烯丙基溴格氏试剂溶液通过以下步骤制成:
在无水无氧条件下,将镁屑和碘置于三口烧瓶中,加入***,降温至0-5℃缓慢滴加烯丙基溴的***溶液,滴加结束后,0-5℃下反应2h,得到烯丙基溴格氏试剂溶液,镁屑、碘、***和烯丙基溴的***溶液的用量比为3g:0.2-0.25g:50mL:20mL,烯丙基溴的***溶液中烯丙基溴和***的用量比为105mmol:20mL。
6.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,步骤S22中巯基化氧化石墨烯和乙烯基POSS的质量比为1:0.1-0.2。
7.根据权利要求1所述的耐泥耐腐蚀船舶用电缆料,其特征在于,步骤S22中安息香二甲醚用量为巯基化氧化石墨烯和乙烯基POSS质量和的2%。
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