CN114940787A - 一种耐高温不易老化电缆及其制备方法 - Google Patents
一种耐高温不易老化电缆及其制备方法 Download PDFInfo
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- CN114940787A CN114940787A CN202210744547.7A CN202210744547A CN114940787A CN 114940787 A CN114940787 A CN 114940787A CN 202210744547 A CN202210744547 A CN 202210744547A CN 114940787 A CN114940787 A CN 114940787A
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Abstract
本发明公开了一种耐高温不易老化电缆及其制备方法,涉及电缆技术领域。本发明先在电缆基体表面沉积碳酸钙晶须,然后用阳离子淀粉使晶须表面呈正电荷,再通过静电吸引,诱导酸化后的碳纳米管沉积;接着进行热处理,淀粉炭化,同时碳酸钙晶须释放,刺破壳层,形成散热通道,提高电缆的耐高温性能;然后利用紫外辐照,将乙烯基二氯硅烷接枝于聚乙烯表面,并附着于散热通道,形成氮氧化硅,增益电缆的耐高温性能;然后用2‑乙氧基‑1‑甲氧基‑4‑乙烯基苯、2‑氨基‑5‑氟苯乙酸、二硫化碳、氨基癸烷改性聚乙烯,作为抗老化护套料,获得电缆。本发明制备的电缆具有耐高温、抗老化的效果。
Description
技术领域
本发明涉及电缆技术领域,具体为一种耐高温不易老化电缆及其制备方法。
背景技术
电缆作为电能传输的基本介质被广泛应用于工业生产、日常生活、经营活动等人类社会活动中,可以说,由各类电缆密集铺设构建的巨型网络在人类的现代社会中起到了不可替代的重要作用。在我国,电缆行业是重要的工业配套产业,在我国的工业体系中发挥着重要的不可替代的作用。
电缆长时间处于户外环境,面临着长期紫外辐射、臭氧共同侵蚀,导致电缆表面开裂变形,严重影响着使用寿命。此外,目前市场上的聚乙烯电缆的耐热等级一般只有70℃或者90℃,在超出耐热等级的温度下长期工作会大大加快电缆绝缘层的老化速度,使导体暴露在空气中,影响电缆的正常使用,这种缺陷极大地限制了聚乙烯电缆的应用场景。
发明内容
本发明的目的在于提供一种耐高温不易老化电缆及其制备方法,以解决现有技术中存在的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种耐高温不易老化电缆,包括电缆基体、耐高温层、屏蔽层、护套层,所述电缆基体包括铜芯层、聚乙烯-氢氧化钙绝缘层;所述护套层由改性聚乙烯制得。
进一步的,所述聚乙烯-氢氧化钙绝缘层按重量份数计,主要包括60~80份线性低密度聚乙烯,10~22份氢氧化钙,5~8份煅烧陶土,2~4份聚乙烯蜡,1~3份促进剂TMTD,0.6~2份乙烯基三乙氧基硅烷。
进一步的,耐高温层由以下方法制得,将电缆基体置于柠檬酸溶液中,碳酸铵气氛下密封静置后,捞出、洗涤,再置于氯化镁溶液中,通入碳酸铵和二氧化碳,陈化得含碳酸钙基体;将含碳酸钙基体置于阳离子淀粉乳液,超声处理得淀粉基体;将淀粉基体置于碳纳米管分散液,超声处理后,捞出、洗涤,然后加热、保温、冷却得复合碳基体;将复合碳基体与乙烯基二氯硅烷混合,紫外辐照后得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶混合,搅拌反应后,在氨气氛围下,继续反应,捞出、洗涤,再置于正丁醚,加热、保温得耐高温层电缆。
进一步的,所述改性聚乙烯由线性低密度聚乙烯、2-乙氧基-1-甲氧基-4-乙烯基苯、2-氨基-5-氟苯乙酸、二硫化碳、氨基癸烷制得。
进一步,一种耐高温不易老化电缆的制备方法,包括以下制备步骤:
(1)将电缆基体置于电缆基体质量1~4倍的柠檬酸溶液中,在碳酸铵气氛下,密封静置20~26h后,捞出,用去离子水洗涤3~7次,再置于电缆基体质量0.8~3.0倍的氯化镁溶液,按流量比1:1~1:3通入碳酸铵和二氧化碳,80~90℃、30~40kHz下陈化0.5~3h后,捞出,置于0~5℃的蒸馏水中,冷却15~30min后,捞出,90~105℃下干燥12~18h得含碳酸钙基体;
(2)86~100℃下,将含碳酸钙基体置于含碳酸钙基体质量0.2~0.5倍的阳离子淀粉乳液,30~40kHz下超声10~24min后,捞出,常温干燥24~30h得淀粉基体;将淀粉基体置于淀粉基体质量7~17倍的碳纳米管分散液,30~40kHz下超声18~26h后,捞出,用去离子水洗涤3~5次后,升温至150~170℃,保温2~6h,然后在氮气氛围下,继续升温至760~800℃,保温40~60min后,冷却至室温,用去离子水冲洗3~6min,得复合碳基体;
(3)将复合碳基体、二苯甲酮、乙烯基二氯硅烷、无水乙醇按质量比1:0.005:0.2:3~1:0.01:0.5:9混合,紫外辐照10~30min后,捞出,用无水乙醇洗涤4~6次,60~78℃干燥5~10h得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶按质量比1:8~1:12混合,40~70rpm下搅拌1~4h后,在氨气氛围下,反应1.5~3h后,捞出,用去离子水洗涤4~8min,再置于硅氮聚合物前驱体质量3~6倍的正丁醚,升温至100~120℃,保温1~4h,继续升温至290~360℃,保温1~3h后,冷却至室温,捞出,依次用丙酮、去离子水洗涤4~8次,得耐高温层电缆;
(4)将线性低密度聚乙烯热压成1mm厚片材,再与二苯甲酮、2-乙氧基-1-甲氧基-4-乙烯基苯、无水乙醇按质量比1:0.002:0.1:3~1:0.01:0.4:9混合,紫外辐照10~30min后,过滤,用无水乙醇洗涤4~6次;再置于线性低密度聚乙烯质量10~18倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量0.8~1.7倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,40~60rpm下搅拌8~18min后,加入线性低密度聚乙烯质量2~4倍的伊顿试剂,继续搅拌26~40min后,室温下继续搅拌30~44min,升温至50~60℃,继续搅拌10~14h,冷却至室温,过滤得二苯甲酮化合物;
(5)将二苯甲酮化合物、氨基癸烷加入环己胺、蒸馏水按质量比1:0.8:5~1:1.6:9混合,以0.1~0.2mL/min滴加二苯甲酮化合物质量0.2~0.5倍的二硫化碳,40~50℃下反应2~5h后,降至室温,过滤,用蒸馏水洗涤3~5次,70~80℃干燥2~4h得硫脲化合物;
(6)将硫脲化合物置于硫脲化合物质量120~139倍的二氯甲烷,氮气保护下,置于冰浴中,40~60rpm下搅拌8~22min,再加入硫脲化合物质量25~31倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌30~45min,然后于室温下反应4~7h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为8~9,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为4~5,依次用乙酸乙酯、去离子水洗涤4~6次,得羟基化合物;
(7)将羟基化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:11:0.8:1.0:2.1~1:18:1.3:1.5:2.8混合,搅拌均匀后,反应3~6h,再加入羟基化合物质量22~34倍的饱和碳酸氢钠溶液,混合均匀后,静置20~42min,过滤,用饱和食盐水洗涤4~7次,50~60℃干燥6~10h得改性聚乙烯;
(8)将改性聚乙烯、炭黑、偶联剂KH560、促进剂NA-22、邻苯二甲酸二丁酯和聚乙烯蜡按质量比1:0.1:0.02:0.01:0.05:0.02~1:0.3:0.04:0.04:0.06:0.06混合,搅拌均匀后,145~165℃下混炼、造粒,得护套料;向耐高温层电缆编织厚为0.1~0.4mm的铜屏蔽层,再挤出护套层,得耐高温不易老化电缆。
进一步,步骤(1)所述柠檬酸溶液的制备方法为,将柠檬酸和去离子水按质量比1:25~1:40混合,加入质量分数为5%的氢氧化钠至溶液pH为4~4.5;所述氯化镁溶液为氯化镁和去离子水按质量比1:28~1:42混合。
进一步,步骤(2)所述阳离子淀粉乳液的具体制备方法为:将阳离子淀粉溶于阳离子淀粉质量1.0~2.4倍的蒸馏水,混合均匀后,82~95℃水浴加热至完全成糊后,常温冷却105~120min,60~100rpm下搅拌15~37min。
进一步,步骤(2)所述碳纳米管分散液的具体制备方法为:将碳纳米管浸泡在碳纳米管质量1~4倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,100~116℃、120~150rpm下搅拌1~3h后,加入去离子水至溶液pH为5~6,30~40kHz下超声分散50~66min,10000~13000rpm下离心处理6~20min,取上清液。
进一步,步骤(3)、(4)所述紫外辐照条件为800~900mJ/cm-2。
进一步,步骤(8)所述挤出过程中各区间温度分别为125~140℃、130~150℃、150~165℃、155~170℃、160~175℃、160~175℃、155~170℃。
与现有技术相比,本发明所达到的有益效果是:
本发明依次在电缆基体表面制备耐高温层、护套层,以实现耐高温、防老化的效果。
首先,本发明先在电缆基体表面沉积碳酸钙晶须,表面聚乙烯绝缘层掺杂氢氧化钙,柠檬酸利用负电荷的羧酸根,捕捉表面钙离子,以形成晶须成核的模板,从而与气相碳酸铵接触,表面形成碳酸钙沉积,并且在氯化镁的作用下,形成氢氧化镁附着在碳酸钙表面,有效调控碳酸钙晶须生长;然后用阳离子淀粉颗粒均匀包覆在碳酸钙晶须表面,同时连接各晶须,形成交联网络结构,再通过静电吸引,诱导酸化后的碳纳米管沉积于碳酸钙晶须表面;接着进行热处理,淀粉颗粒炭化形成炭层,同时碳酸钙晶须经高温分解释放出大量二氧化碳,刺破淀粉炭层和碳纳米管产生大量贯通的微孔,形成散热通道,提高电缆的耐高温性能;然后利用紫外辐照,引发聚乙烯绝缘层与乙烯基二氯硅烷的自由基反应,使其接枝于电缆基体表面,再与吡啶络合、氨解,附着于散热通道,形成硅氮聚合物,并进一步热氧化分解,形成耐高温的氮氧化硅,增益电缆的耐高温性能。
其次,护套层采用改性聚乙烯为原料;先利用紫外辐照,将2-乙氧基-1-甲氧基-4-乙烯基苯接枝于聚乙烯中,形成侧链,芳基与2-氨基-5-氟苯乙酸的羧基反应,形成抗紫外基团二苯甲酮,使电缆具有抗紫外老化性能,氨基与二硫化碳进行亲核加成反应,形成异硫氰基团,再与氨基癸烷的氨基继续反应,形成硫脲基团,使电缆具有抗臭氧老化效果;接着将乙氧基和甲氧基还原成羟基,羟基与氨基癸烷的氨基反应,从而使侧链外端为疏水长链,防止护套层与水分接触,增益电缆的抗老化效果。
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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
为了更清楚的说明本发明提供的方法通过以下实施例进行详细说明,在以下实施例中制作的耐高温不易老化电缆的各指标测试方法如下:
耐高温性、抗紫外老化:取相同大小的实施例与对比例进行耐高温、光老化效果测试,参照GB/T8815测量断裂伸长率、拉伸强度的最大变化率,其中测试条件分别为为150℃下放置168h,0.45W/m2、340nm紫外光老化6000h。
抗臭氧老化性:取相同大小的实施例与对比例进行臭氧老化效果测试,将试样置于臭氧浓度0.025%、26℃的环境下,放置50h,观察表面有无开裂现象。
实施例1
(1)将柠檬酸和去离子水按质量比1:25混合,加入质量分数为5%的氢氧化钠至溶液pH为4,得柠檬酸溶液;将电缆基体置于电缆基体质量1倍的柠檬酸溶液中,在碳酸铵气氛下,密封静置20h后,捞出,用去离子水洗涤3次,再置于电缆基体质量0.8倍的氯化镁溶液,氯化镁溶液中氯化镁和去离子水的质量比为1:28,按流量比1:1通入碳酸铵和二氧化碳,80℃、30kHz下陈化0.5h后,捞出,置于0℃的蒸馏水中,冷却15min后,捞出,90℃下干燥12h得含碳酸钙基体;
(2)将阳离子淀粉溶于阳离子淀粉质量1倍的蒸馏水,混合均匀后,82℃水浴加热至完全成糊后,常温冷却105min,60rpm下搅拌15min,得阳离子淀粉乳液;86℃下,将含碳酸钙基体置于含碳酸钙基体质量0.2倍的阳离子淀粉乳液,30kHz下超声10min后,捞出,常温干燥24h得淀粉基体;将碳纳米管浸泡在碳纳米管质量1倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,100℃、120rpm下搅拌1h后,加入去离子水至溶液pH为5,30kHz下超声分散50min,10000rpm下离心处理6min,取上清液,得碳纳米管分散液;将淀粉基体置于淀粉基体质量7倍的碳纳米管分散液,30kHz下超声18h后,捞出,用去离子水洗涤3次后,升温至150℃,保温2h,然后在氮气氛围下,继续升温至760℃,保温40min后,冷却至室温,用去离子水冲洗3min,得复合碳基体;
(3)将复合碳基体、二苯甲酮、乙烯基二氯硅烷、无水乙醇按质量比1:0.005:0.2:3混合,800mJ/cm-2下辐照10min后,捞出,用无水乙醇洗涤4次,60℃干燥5h得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶按质量比1:8混合,40rpm下搅拌1h后,在氨气氛围下,反应1.5h后,捞出,用去离子水洗涤4min,再置于硅氮聚合物前驱体质量3倍的正丁醚,升温至100℃,保温1h,继续升温至290℃,保温1h后,冷却至室温,捞出,依次用丙酮、去离子水洗涤4次,得耐高温层电缆;
(4)将线性低密度聚乙烯热压成1mm厚片材,再与二苯甲酮、2-乙氧基-1-甲氧基-4-乙烯基苯、无水乙醇按质量比1:0.002:0.1:3混合,800mJ/cm-2下辐照10min后,过滤,用无水乙醇洗涤4次;再置于线性低密度聚乙烯质量10倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量0.8倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,40rpm下搅拌8min后,加入线性低密度聚乙烯质量2倍的伊顿试剂,继续搅拌26min后,室温下继续搅拌30min,升温至50℃,继续搅拌10h,冷却至室温,过滤得二苯甲酮化合物;
(5)将二苯甲酮化合物、氨基癸烷加入环己胺、蒸馏水按质量比1:0.8:5混合,以0.1mL/min滴加二苯甲酮化合物质量0.2倍的二硫化碳,40℃下反应2h后,降至室温,过滤,用蒸馏水洗涤3次,70℃干燥2h得硫脲化合物;
(6)将硫脲化合物置于硫脲化合物质量120倍的二氯甲烷,氮气保护下,置于冰浴中,40rpm下搅拌8min,再加入硫脲化合物质量25倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌30min,然后于室温下反应4h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为8,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为4,依次用乙酸乙酯、去离子水洗涤4次,得羟基化合物;
(7)将羟基化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:11:0.8:1.0:2.1混合,搅拌均匀后,反应3h,再加入羟基化合物质量22倍的饱和碳酸氢钠溶液,混合均匀后,静置20min,过滤,用饱和食盐水洗涤4次,50℃干燥6h得改性聚乙烯;
(8)将改性聚乙烯、炭黑、偶联剂KH560、促进剂NA-22、邻苯二甲酸二丁酯和聚乙烯蜡按质量比1:0.1:0.02:0.01:0.05:0.02混合,搅拌均匀后,145℃下混炼、造粒,得护套料;向耐高温层电缆编织厚为0.1mm的铜屏蔽层,再挤出护套层,各区间温度分别为125℃、130℃、150℃、155℃、160℃、160℃、155℃,得耐高温不易老化电缆。
实施例2
(1)将柠檬酸和去离子水按质量比1:32.5混合,加入质量分数为5%的氢氧化钠至溶液pH为4.25,得柠檬酸溶液;将电缆基体置于电缆基体质量2.5倍的柠檬酸溶液中,在碳酸铵气氛下,密封静置23h后,捞出,用去离子水洗涤5次,再置于电缆基体质量1.9倍的氯化镁溶液,氯化镁溶液中氯化镁和去离子水的质量比为1:35,按流量比1:2通入碳酸铵和二氧化碳,85℃、35kHz下陈化1.7h后,捞出,置于2℃的蒸馏水中,冷却22min后,捞出,97℃干燥15h得含碳酸钙基体;
(2)将阳离子淀粉溶于阳离子淀粉质量1.7倍的蒸馏水,混合均匀后,88℃水浴加热至完全成糊后,常温冷却112min,80rpm下搅拌26min,得阳离子淀粉乳液;93℃下,将含碳酸钙基体置于含碳酸钙基体质量0.35倍的阳离子淀粉乳液,35kHz下超声17min后,捞出,常温干燥27h得淀粉基体;将碳纳米管浸泡在碳纳米管质量2.5倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,108℃、130rpm下搅拌2h后,加入去离子水至溶液pH为5.5,35kHz下超声分散58min,12000rpm下离心处理13min,取上清液,得碳纳米管分散液;将淀粉基体置于淀粉基体质量12倍的碳纳米管分散液,35kHz下超声22h后,捞出,用去离子水洗涤4次后,升温至160℃,保温4h,然后在氮气氛围下,继续升温至780℃,保温50min后,冷却至室温,用去离子水冲洗4min,得复合碳基体;
(3)将复合碳基体、二苯甲酮、乙烯基二氯硅烷、无水乙醇按质量比1:0.0075:0.35:6混合,850mJ/cm-2下辐照20min后,捞出,用无水乙醇洗涤5次,69℃干燥7.5h得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶按质量比1:10混合,60rpm下搅拌2.5h后,在氨气氛围下,反应2.2h后,捞出,用去离子水洗涤6min,再置于硅氮聚合物前驱体质量4.5倍的正丁醚,升温至110℃,保温2.5h,继续升温至325℃,保温2h后,冷却至室温,捞出,依次用丙酮、去离子水洗涤6次,得耐高温层电缆;
(4)将线性低密度聚乙烯热压成1mm厚片材,再与二苯甲酮、2-乙氧基-1-甲氧基-4-乙烯基苯、无水乙醇按质量比1:0.006:0.25:6混合,850mJ/cm-2下辐照20min后,过滤,用无水乙醇洗涤5次;再置于线性低密度聚乙烯质量14倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量1.25倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,50rpm下搅拌13min后,加入线性低密度聚乙烯质量3倍的伊顿试剂,继续搅拌33min后,室温下继续搅拌37min,升温至55℃,继续搅拌12h,冷却至室温,过滤得二苯甲酮化合物;
(5)将二苯甲酮化合物、氨基癸烷加入环己胺、蒸馏水按质量比1:1.2:7混合,以0.15mL/min滴加二苯甲酮化合物质量0.35倍的二硫化碳,45℃下反应3.5h后,降至室温,过滤,用蒸馏水洗涤4次,75℃干燥3h得硫脲化合物;
(6)将硫脲化合物置于硫脲化合物质量129.5倍的二氯甲烷,氮气保护下,置于冰浴中,50rpm下搅拌15min,再加入硫脲化合物质量28倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌37min,然后于室温下反应5.5h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为8.5,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为4.5,依次用乙酸乙酯、去离子水洗涤5次,得羟基化合物;
(7)将羟基化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:14.5:1.05:1.25:2.45混合,搅拌均匀后,反应4.5h,再加入羟基化合物质量28倍的饱和碳酸氢钠溶液,混合均匀后,静置31min,过滤,用饱和食盐水洗涤6次,55℃干燥8h得改性聚乙烯;
(8)将改性聚乙烯、炭黑、偶联剂KH560、促进剂NA-22、邻苯二甲酸二丁酯和聚乙烯蜡按质量比1:0.2:0.03:0.025:0.055:0.04混合,搅拌均匀后,155℃下混炼、造粒,得护套料;向耐高温层电缆编织厚为0.25mm的铜屏蔽层,再挤出护套层,各区间温度分别为132℃、140℃、158℃、162℃、168℃、168℃、162℃,得耐高温不易老化电缆。
实施例3
(1)将柠檬酸和去离子水按质量比1:40混合,加入质量分数为5%的氢氧化钠至溶液pH为4.5,得柠檬酸溶液;将电缆基体置于电缆基体质量4倍的柠檬酸溶液中,在碳酸铵气氛下,密封静置26h后,捞出,用去离子水洗涤7次,再置于电缆基体质量3.0倍的氯化镁溶液,氯化镁溶液中氯化镁和去离子水的质量比为1:42,按流量比1:3通入碳酸铵和二氧化碳,90℃、40kHz下陈化3h后,捞出,置于5℃的蒸馏水中,冷却30min后,捞出,105℃干燥18h得含碳酸钙基体;
(2)将阳离子淀粉溶于阳离子淀粉质量2.4倍的蒸馏水,混合均匀后,95℃水浴加热至完全成糊后,常温冷却120min,100rpm下搅拌37min,得阳离子淀粉乳液;100℃下,将含碳酸钙基体置于含碳酸钙基体质量0.5倍的阳离子淀粉乳液,40kHz下超声24min后,捞出,常温干燥30h得淀粉基体;将碳纳米管浸泡在碳纳米管质量4倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,116℃、150rpm下搅拌3h后,加入去离子水至溶液pH为6,40kHz下超声分散66min,13000rpm下离心处理20min,取上清液,得碳纳米管分散液;将淀粉基体置于淀粉基体质量17倍的碳纳米管分散液,40kHz下超声26h后,捞出,用去离子水洗涤5次后,升温至170℃,保温6h,然后在氮气氛围下,继续升温至800℃,保温60min后,冷却至室温,用去离子水冲洗6min,得复合碳基体;
(3)将复合碳基体、二苯甲酮、乙烯基二氯硅烷、无水乙醇按质量比1:0.01:0.5:9混合,900mJ/cm-2下辐照30min后,捞出,用无水乙醇洗涤6次,78℃干燥10h得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶按质量比1:12混合,70rpm下搅拌4h后,在氨气氛围下,反应3h后,捞出,用去离子水洗涤8min,再置于硅氮聚合物前驱体质量6倍的正丁醚,升温至120℃,保温4h,继续升温至360℃,保温3h后,冷却至室温,捞出,依次用丙酮、去离子水洗涤8次,得耐高温层电缆;
(4)将线性低密度聚乙烯热压成1mm厚片材,再与二苯甲酮、2-乙氧基-1-甲氧基-4-乙烯基苯、无水乙醇按质量比1:0.01:0.4:9混合,900mJ/cm-2下辐照30min后,过滤,用无水乙醇洗涤6次;再置于线性低密度聚乙烯质量18倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量1.7倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,60rpm下搅拌18min后,加入线性低密度聚乙烯质量4倍的伊顿试剂,继续搅拌40min后,室温下继续搅拌44min,升温至60℃,继续搅拌14h,冷却至室温,过滤得二苯甲酮化合物;
(5)将二苯甲酮化合物、氨基癸烷加入环己胺、蒸馏水按质量比1:1.6:9混合,以0.2mL/min滴加二苯甲酮化合物质量0.5倍的二硫化碳,50℃下反应5h后,降至室温,过滤,用蒸馏水洗涤5次,80℃干燥4h得硫脲化合物;
(6)将硫脲化合物置于硫脲化合物质量139倍的二氯甲烷,氮气保护下,置于冰浴中,60rpm下搅拌22min,再加入硫脲化合物质量31倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌45min,然后于室温下反应7h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为9,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为5,依次用乙酸乙酯、去离子水洗涤6次,得羟基化合物;
(7)将羟基化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:18:1.3:1.5:2.8混合,搅拌均匀后,反应6h,再加入羟基化合物质量34倍的饱和碳酸氢钠溶液,混合均匀后,静置42min,过滤,用饱和食盐水洗涤7次,60℃干燥10h得改性聚乙烯;
(8)将改性聚乙烯、炭黑、偶联剂KH560、促进剂NA-22、邻苯二甲酸二丁酯和聚乙烯蜡按质量比1:0.3:0.04:0.04:0.06:0.06混合,搅拌均匀后,165℃下混炼、造粒,得护套料;向耐高温层电缆编织厚为0.4mm的铜屏蔽层,再挤出护套层,各区间温度分别为140℃、150℃、165℃、170℃、175℃、175℃、170℃,得耐高温不易老化电缆。
对比例1
对比例1与实施例2的区别在于无步骤(1),其余步骤同实施例2。
对比例2
对比例2与实施例2的区别在于步骤(2)的不同,将步骤(2)改为:将碳纳米管浸泡在碳纳米管质量2.5倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,108℃、130rpm下搅拌2h后,加入去离子水至溶液pH为5.5,35kHz下超声分散58min,12000rpm下离心处理13min,取上清液,得碳纳米管分散液;将含碳酸钙基体置于含碳酸钙基体质量12倍的碳纳米管分散液,35kHz下超声22h后,捞出,用去离子水洗涤4次后,升温至160℃,保温4h,然后在氮气氛围下,继续升温至780℃,保温50min后,冷却至室温,用去离子水冲洗4min,得复合碳基体。其余步骤同实施例2。
对比例3
对比例3与实施例2的区别在于无步骤(3),其余步骤同实施例2。
对比例4
对比例4与实施例2的区别在于步骤(4)不同,将步骤(4)改为:将线性低密度聚乙烯热压成1mm厚片材,置于线性低密度聚乙烯质量14倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量1.25倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,50rpm下搅拌13min后,加入线性低密度聚乙烯质量3倍的伊顿试剂,继续搅拌33min后,室温下继续搅拌37min,升温至55℃,继续搅拌12h,冷却至室温,过滤得二苯甲酮化合物。其余步骤同实施例2。
对比例5
对比例5与实施例2的区别在于无步骤(5),步骤(6)改为:将二苯甲酮化合物置于二苯甲酮化合物质量129.5倍的二氯甲烷,氮气保护下,置于冰浴中,50rpm下搅拌15min,再加入二苯甲酮化合物质量28倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌37min,然后于室温下反应5.5h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为8.5,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为4.5,依次用乙酸乙酯、去离子水洗涤5次,得羟基化合物。其余步骤同实施例2。
对比例6
对比例6与实施例2的区别在于无步骤(6),步骤(7)改为:将硫脲化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:14.5:1.05:1.25:2.45混合,搅拌均匀后,反应4.5h,再加入硫脲化合物质量28倍的饱和碳酸氢钠溶液,混合均匀后,静置31min,过滤,用饱和食盐水洗涤6次,55℃干燥8h得改性聚乙烯。其余步骤同实施例2。
效果例
下表1给出了采用本发明实施例1至3与对比例1至6的耐高温不易老化电缆的性能分析结果。
表1
从实施例与对比例的150℃下断裂伸长率、拉伸轻度最大变化率的实验数据对比可发现,本发明在电缆基体表面沉积碳酸钙晶须,提供中空孔道模板,并利用阳离子淀粉颗粒改性碳酸钙,使表面呈正电荷,同时连接各晶须,形成交联网络结构,再酸化碳纳米管,呈负电荷,通过静电吸引,沉积于碳酸钙晶须表面;然后淀粉颗粒炭化形成炭层,同时碳酸钙晶须释放出大量二氧化碳,刺破壳层产生贯通的微孔,形成散热通道,提高电缆的耐高温性能;然后利用紫外辐照,使乙烯基二氯硅烷接枝于聚乙烯表面,附着于散热通道,形成氮氧化硅,增益电缆的耐高温性能;从实施例与对比例的紫外光下断裂伸长率、拉伸轻度最大变化率、臭氧老化后表面情况的实验数据对比可发现,利用2-乙氧基-1-甲氧基-4-乙烯基苯、2-氨基-5-氟苯乙改性聚乙烯,形成二苯甲酮侧链,使电缆具有抗紫外老化性能,再与二硫化碳、氨基癸烷继续反应,形成硫脲基团,使电缆具有抗臭氧老化效果;接着将侧链外端变为疏水长链,增益电缆的抗老化效果。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
Claims (10)
1.一种耐高温不易老化电缆,包括电缆基体、耐高温层、屏蔽层、护套层,其特征在于,所述电缆基体包括铜芯层、聚乙烯-氢氧化钙绝缘层;所述护套层由改性聚乙烯制得。
2.根据权利要求1所述的一种耐高温不易老化电缆,其特征在于,所述聚乙烯-氢氧化钙绝缘层按重量份数计,主要包括60~80份线性低密度聚乙烯,10~22份氢氧化钙,5~8份煅烧陶土,2~4份聚乙烯蜡,1~3份促进剂TMTD,0.6~2份乙烯基三乙氧基硅烷。
3.根据权利要求1所述的一种耐高温不易老化电缆,其特征在于,所述耐高温层由以下方法制得,将电缆基体置于柠檬酸溶液中,碳酸铵气氛下密封静置后,捞出、洗涤,再置于氯化镁溶液中,通入碳酸铵和二氧化碳,陈化得含碳酸钙基体;将含碳酸钙基体置于阳离子淀粉乳液,超声处理得淀粉基体;将淀粉基体置于碳纳米管分散液,超声处理后,捞出、洗涤,然后加热、保温、冷却得复合碳基体;将复合碳基体与乙烯基二氯硅烷混合,紫外辐照后得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶混合,搅拌反应后,在氨气氛围下,继续反应,捞出、洗涤,再置于正丁醚,加热、保温得耐高温层电缆。
4.根据权利要求1所述的一种耐高温不易老化电缆,其特征在于,所述改性聚乙烯由线性低密度聚乙烯、2-乙氧基-1-甲氧基-4-乙烯基苯、2-氨基-5-氟苯乙酸、二硫化碳、氨基癸烷制得。
5.一种耐高温不易老化电缆的制备方法,其特征在于,包括以下制备步骤:
(1)将电缆基体置于电缆基体质量1~4倍的柠檬酸溶液中,在碳酸铵气氛下,密封静置20~26h后,捞出,用去离子水洗涤3~7次,再置于电缆基体质量0.8~3.0倍的氯化镁溶液,按流量比1:1~1:3通入碳酸铵和二氧化碳,80~90℃、30~40kHz下陈化0.5~3h后,捞出,置于0~5℃的蒸馏水中,冷却15~30min后,捞出,90~105℃下干燥12~18h,得含碳酸钙基体;
(2)86~100℃下,将含碳酸钙基体置于含碳酸钙基体质量0.2~0.5倍的阳离子淀粉乳液,30~40kHz下超声10~24min后,捞出,常温干燥24~30h得淀粉基体;将淀粉基体置于淀粉基体质量7~17倍的碳纳米管分散液,30~40kHz下超声18~26h后,捞出,用去离子水洗涤3~5次后,升温至150~170℃,保温2~6h,然后在氮气氛围下,继续升温至760~800℃,保温40~60min后,冷却至室温,用去离子水冲洗3~6min,得复合碳基体;
(3)将复合碳基体、二苯甲酮、乙烯基二氯硅烷、无水乙醇按质量比1:0.005:0.2:3~1:0.01:0.5:9混合,紫外辐照10~30min后,捞出,用无水乙醇洗涤4~6次,60~78℃干燥5~10h得硅氮聚合物前驱体;将硅氮聚合物前驱体、吡啶按质量比1:8~1:12混合,40~70rpm下搅拌1~4h后,在氨气氛围下,反应1.5~3h后,捞出,用去离子水洗涤4~8min,再置于硅氮聚合物前驱体质量3~6倍的正丁醚,升温至100~120℃,保温1~4h,继续升温至290~360℃,保温1~3h后,冷却至室温,捞出,依次用丙酮、去离子水洗涤4~8次,得耐高温层电缆;
(4)将线性低密度聚乙烯热压成1mm厚片材,再与二苯甲酮、2-乙氧基-1-甲氧基-4-乙烯基苯、无水乙醇按质量比1:0.002:0.1:3~1:0.01:0.4:9混合,紫外辐照10~30min后,过滤,用无水乙醇洗涤4~6次;再置于线性低密度聚乙烯质量10~18倍的1,2-二氯乙烷,混合均匀后,加入线性低密度聚乙烯质量0.8~1.7倍的2-氨基-5-氟苯乙酸,氩气保护下,置于冰浴中,40~60rpm下搅拌8~18min后,加入线性低密度聚乙烯质量2~4倍的伊顿试剂,继续搅拌26~40min后,室温下继续搅拌30~44min,升温至50~60℃,继续搅拌10~14h,冷却至室温,过滤得二苯甲酮化合物;
(5)将二苯甲酮化合物、氨基癸烷加入环己胺、蒸馏水按质量比1:0.8:5~1:1.6:9混合,以0.1~0.2mL/min滴加二苯甲酮化合物质量0.2~0.5倍的二硫化碳,40~50℃下反应2~5h后,降至室温,过滤,用蒸馏水洗涤3~5次,70~80℃干燥2~4h得硫脲化合物;
(6)将硫脲化合物置于硫脲化合物质量120~139倍的二氯甲烷,氮气保护下,置于冰浴中,40~60rpm下搅拌8~22min,再加入硫脲化合物质量25~31倍的三溴化硼溶液,三溴化硼溶液中三溴化硼和二氯甲烷的质量比为17:100,继续搅拌30~45min,然后于室温下反应4~7h,加入甲醇至无烟雾挥发,再加入质量分数为15%的氢氧化钠至溶液pH为8~9,过滤得滤体;用质量分数为10%的盐酸洗涤滤体至表面pH为4~5,依次用乙酸乙酯、去离子水洗涤4~6次,得羟基化合物;
(7)将羟基化合物、N,N-二甲基甲酰胺、氨基癸烷、N,N-二异丙基乙胺、2-(7-氧化苯并三氮唑)-N,N,N',N'-四甲基脲六氟磷酸酯按质量比1:11:0.8:1.0:2.1~1:18:1.3:1.5:2.8混合,搅拌均匀后,反应3~6h,再加入羟基化合物质量22~34倍的饱和碳酸氢钠溶液,混合均匀后,静置20~42min,过滤,用饱和食盐水洗涤4~7次,50~60℃干燥6~10h得改性聚乙烯;
(8)将改性聚乙烯、炭黑、偶联剂KH560、促进剂NA-22、邻苯二甲酸二丁酯和聚乙烯蜡按质量比1:0.1:0.02:0.01:0.05:0.02~1:0.3:0.04:0.04:0.06:0.06混合,搅拌均匀后,145~165℃下混炼、造粒,得护套料;向耐高温层电缆编织厚为0.1~0.4mm的铜屏蔽层,再挤出护套层,得耐高温不易老化电缆。
6.根据权利要求5所述的一种耐高温不易老化电缆的制备方法,其特征在于,步骤(1)所述柠檬酸溶液的制备方法为,将柠檬酸和去离子水按质量比1:25~1:40混合,加入质量分数为5%的氢氧化钠至溶液pH为4~4.5;所述氯化镁溶液为氯化镁和去离子水按质量比1:28~1:42混合。
7.根据权利要求5所述的一种耐高温不易老化电缆的制备方法,其特征在于,步骤(2)所述阳离子淀粉乳液的具体制备方法为:将阳离子淀粉溶于阳离子淀粉质量1.0~2.4倍的蒸馏水,混合均匀后,82~95℃水浴加热至完全成糊后,常温冷却105~120min,60~100rpm下搅拌15~37min。
8.根据权利要求5所述的一种耐高温不易老化电缆的制备方法,其特征在于,步骤(2)所述碳纳米管分散液的具体制备方法为:将碳纳米管浸泡在碳纳米管质量1~4倍的酸混合液,酸混合液中质量分数为70%的硫酸、质量分数为68%的硝酸的质量比为3.94:1,100~116℃、120~150rpm下搅拌1~3h后,加入去离子水至溶液pH为5~6,30~40kHz下超声分散50~66min,10000~13000rpm下离心处理6~20min,取上清液。
9.根据权利要求5所述的一种耐高温不易老化电缆的制备方法,其特征在于,步骤(3)、(4)所述紫外辐照条件为800~900mJ/cm-2。
10.根据权利要求5所述的一种耐高温不易老化电缆的制备方法,其特征在于,步骤(8)所述挤出过程中各区间温度分别为125~140℃、130~150℃、150~165℃、155~170℃、160~175℃、160~175℃、155~170℃。
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