CN113603969B - 一种具有耐热性能的mpp电力管制备方法 - Google Patents
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Abstract
本发明公开了一种具有耐热性能的MPP电力管制备方法,涉及电力管领域,包括电力管耐热层、电力管阻燃层和应力层,将2,6‑二叔丁基苯酚加入到三口烧瓶中,将多聚甲醛和催化剂滴加入三口瓶中,得到中间体A,将双酚B和无水碳酸钾加入到三口瓶中,加入亚磷酸三乙酯,得到中间体B,将中间体A和催化剂加入到三口瓶中,加入中间体B,得到该抗氧化剂,解决了现有的MPP电力管易发生氧化变脆和不具备阻燃性能的问题;在高温时分解成N2、NO,NO2等不燃气体,可以稀释空气中的氧气和聚合物受热分解产生的可燃物的浓度,且分解产生的氮的氧化物能捕捉自由基,抑制高聚物的链锁反应,从而达到了阻燃的目的。
Description
技术领域
本发明涉及电力管领域,具体涉及一种具有耐热性能的MPP电力管制备方法。
背景技术
随着城市建设的发展,非开挖技术在的推广和应用也与时俱进,非开挖施工已深入到天然气、上水、下水、污水、电力和信息等地下管线的铺设和修复中,未来几年有望将所有的空中“蜘蛛网”入地,采用地下埋设电缆传输电力,一种用于非开挖用的改性聚丙烯(MPP)塑料顶管作为保护电缆用的塑料护套管正大量的用于工程中,MPP管材比常用HDPE管相比性能更优越,热熔焊接接头柔性好、焊接头强度高、耐温性能好,可用作超长度高牵引力拖管,具有优良的抗地层沉降以及抗震性能。
MPP电力管在随着应用的扩大,从而得到了全面推广,面对21世纪塑料管需求的大好局面,MPP电力管的发展必有十分广阔的前景,而对于MPP电力管的性能要求也越来越高,现有的MPP电力管易发生氧化变脆,使管道使用寿命缩短,且不具备阻燃性能。
为此,我们提出一种具有耐热性能的MPP电力管制备方法。
发明内容
为了克服上述的技术问题,本发明的目的在于提供了一种具有耐热性能的MPP电力管制备方法:
(1)将2,6-二叔丁基苯酚加入到三口烧瓶中,将多聚甲醛和催化剂装入锥形瓶中,倒入滴液漏斗中,滴加入三口瓶中,得到中间体A,将双酚B和无水碳酸钾加入到三口瓶中,加入亚磷酸三乙酯,得到中间体B,将中间体A和催化剂加入到三口瓶中,加入中间体B,得到抗氧化剂,通过加入该抗氧化剂解决了现有的MPP电力管易发生氧化变脆,使管道使用寿命缩短的问题;
(2)向三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,得到中间体C,向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,得到中间体D,向三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,将中间体D滴加到三口瓶中,得到该电力管阻燃层材料,通过该电力管阻燃层材料的制备解决了现有的MPP电力管不具备阻燃性能的问题。
本发明的目的可以通过以下技术方案实现:
一种具有耐热性能的MPP电力管制备方法,包括电力管耐热层、电力管阻燃层和应力层,所述电力管耐热层的内层设置有应力层,所述应力层的内层设置有电力管阻燃层,具有耐热性能的MPP电力管制备方法包括如下过程:
S1:按重量份分别称取60-70份的聚丙烯、10-30份的玻璃纤维、2-4份的硅烷偶联剂、1-5份的硬脂酸、1-3份的石蜡和1-2份的抗氧化剂混合均匀,得到电力管耐热层共混料;
S2:制备电力管阻燃层材料;
S3:将S1和S2中制备的电力管耐热层共混料和电力管阻燃层材料分别加入到不同料仓干燥预热,经单螺杆挤出机挤出;
S4:采用双层共挤方式,经单螺杆挤出机挤出电力管耐热层和电力管阻燃层,物料由挤出机螺杆加热、熔融、塑化输送到机头口模;
S5:在单螺杆挤出机中加入重量比例为1:3的玻璃纤维和聚乙烯混合而成的中间应力层,通过共挤的方式使电力管耐热层和电力管阻燃层中间形成应力层。
作为本发明进一步的方案:步骤S1中所述抗氧化剂的制备步骤如下:
S21:将2,6-二叔丁基苯酚加入到装有电动搅拌器、氮气导管、温度计的三口烧瓶中,然后通入氮气吹扫,除去反应器中的氧气,反应温度用水浴控制,将多聚甲醛和催化剂装入锥形瓶中,把锥形瓶置于磁力搅拌器上,搅拌,控制温度在50-60℃,待多聚甲醛完全解聚后,倒入滴液漏斗中,滴加入三口瓶中,控制滴加速度为1-2滴/s,反应5-6h,关闭氮气,充分震荡后进行减压蒸馏,重结晶,用加热套加热至其完全溶解,冷却,结晶4-8h后,减压抽滤,得到中间体A;
S22:将双酚B和无水碳酸钾加入到三口瓶中,并加入搅拌子,装上温度计,将三口瓶放入带磁力搅拌的油浴锅中,加入亚磷酸三乙酯,连接冷凝装置,开动磁力搅拌升温至120-130℃开始反应,反应3-4h,停止加热,待温度下降后,减压蒸馏,得到中间体B;
S23:将中间体A和催化剂加入到三口瓶中,再加入二甲苯溶剂和搅拌子,将三口瓶放入带磁力搅拌的油浴锅中,装上温度计、恒压漏斗,连接冷凝装置,开动磁力搅拌升温至120-130℃,加入中间体B,反应3-4h后,减压蒸馏,重结晶,过滤,得到该抗氧化剂。
作为本发明进一步的方案:步骤S21中所述催化剂为叔丁醇钾,所述2,6-二叔丁基苯酚与催化剂的用量比为4.0g:0.08g,所述2,6-二叔丁基苯酚与多聚甲醛的摩尔比为1:2.5。
作为本发明进一步的方案:步骤S22中所述双酚B与无水碳酸钾的用量比为1g:0.6g,所述双酚B与亚磷酸三乙酯的摩尔比为1:2.05。
作为本发明进一步的方案:步骤S23中所述催化剂为有机锡,所述中间体B与催化剂的用量比为0.05g:0.8g,所述中间体A与中间体B的摩尔比为4.1:1。
作为本发明进一步的方案:步骤S2中所述电力管阻燃层材料的制备步骤如下:
S61:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,通入氮气,加热至120-130℃,电磁搅拌15-20h,将体系倒入到含有浓盐酸的蒸馏水中,过滤,并用蒸馏水洗涤,得到中间体C;
S62:向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,在搅拌下加热至80-90℃,反应8-10h,旋转蒸发,得到中间体D;
S63:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,通入氮气,搅拌条件下,将中间体D滴加到三口瓶中,控制滴加速度为1-2滴/s,加热至30-40℃,反应24-26h,倒入到含有浓盐酸的蒸馏水中,置于60-70℃的干燥箱真空干燥10-20h,得到该电力管阻燃层材料。
作为本发明进一步的方案:步骤S61中所述均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺、吡啶、浓盐酸和蒸馏水的用量比为3.30g:5.00g:20mL:2mL:5mL:100mL。
作为本发明进一步的方案:步骤S62中所述中间体C与SOCl2的用量比为8.02g:15mL。
作为本发明进一步的方案:步骤S63中所述1,4-丁炔二醇、三乙胺、N,N-二甲基乙酰胺、中间体D、浓盐酸与蒸馏水的用量比为10.00g:3mL:20mL:8.35g:25mL:500mL。
本发明的有益效果:
(1)本发明将2,6-二叔丁基苯酚加入到三口烧瓶中,将多聚甲醛和催化剂装入锥形瓶中,倒入滴液漏斗中,滴加入三口瓶中,得到中间体A,将双酚B和无水碳酸钾加入到三口瓶中,加入亚磷酸三乙酯,得到中间体B,将中间体A和催化剂加入到三口瓶中,加入中间体B,得到该抗氧化剂,该抗氧化剂为受阻酚类抗氧化剂,其在苯环的羟基的两侧有取代基,由于羟基受到空间障碍,H原子容易从分子上脱落下来,与过氧自由基(RO0-)、烷氧自由基(RO-)或羟自由基(-OH)等结合使之失去活性,从而使热氧老化的链反应终止,添加该抗氧化剂可以明显提高材料的耐热性能,使其不易被热氧化,从而达到了抗氧化、耐热的目的;
(2)向三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,得到中间体C,向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,得到中间体D,向三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,将中间体D滴加到三口瓶中,得到该电力管阻燃层材料,该电力管阻燃层材料的阻燃机理是按气相阻燃机理进行的,它在高温时分解成N2、NO和NO2等不燃气体,可以稀释空气中的氧气和聚合物受热分解产生的可燃物的浓度,同时分解过程中会吸热,降低基材表面温度,且分解产生的氮的氧化物能捕捉自由基,抑制高聚物的链锁反应,且该电力管阻燃层材料耐高温,从而达到了阻燃的目的。
附图说明
下面结合附图对本发明做进一步的说明;
图1是本发明中一种具有耐热性能的MPP电力管的整体结构示意图;
图2是本发明中一种具有耐热性能的MPP电力管的侧视图;
图3是本发明中步骤S21的化学反应式;
图4是本发明中步骤S22的化学反应式;
图5是本发明中步骤S23的化学反应式;
图6是本发明中步骤S61的化学反应式;
图7是本发明中步骤S62的化学反应式;
图8是本发明中步骤S63的化学反应式。
图中:1、电力管耐热层;2、电力管阻燃层;3、应力层。
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。
根据图1-3所示,一种具有耐热性能的MPP电力管制备方法,包括电力管耐热层1、电力管阻燃层2和应力层3,电力管耐热层1的内层设置有应力层3,所述应力层3的内层设置有电力管阻燃层2;
实施例1:
本实施例为一种具有耐热性能的MPP电力管,该具有耐热性能的MPP电力管制备方法包括如下过程:
S1:按重量份分别称取60份的聚丙烯、10份的玻璃纤维、4份的硅烷偶联剂、5份的硬脂酸、3份的石蜡和2份的抗氧化剂混合均匀,得到电力管耐热层共混料;
S2:制备电力管阻燃层材料;
S3:将S1和S2中制备的电力管耐热层共混料和电力管阻燃层材料分别加入到不同料仓干燥预热,经单螺杆挤出机挤出;
S4:采用双层共挤方式,经单螺杆挤出机挤出电力管耐热层1和电力管阻燃层2,物料由挤出机螺杆加热、熔融、塑化输送到机头口模;
S5:在单螺杆挤出机中加入重量比例为1:3的玻璃纤维和聚乙烯混合而成的中间应力层3,通过共挤的方式使电力管耐热层1和电力管阻燃层2中间形成应力层3;
步骤S1中抗氧化剂的制备步骤如下:
S21:将2,6-二叔丁基苯酚加入到装有电动搅拌器、氮气导管、温度计的三口烧瓶中,然后通入氮气吹扫,反应温度用水浴控制,将多聚甲醛和催化剂装入锥形瓶中,把锥形瓶置于磁力搅拌器上,搅拌,控制温度在50℃,待多聚甲醛完全解聚后,倒入滴液漏斗中,滴加入三口瓶中,控制滴加速度为1滴/s,反应5h,关闭氮气,充分震荡后进行减压蒸馏,重结晶,用加热套加热至其完全溶解,冷却,结晶4h后,减压抽滤,得到中间体A;
S22:将双酚B和无水碳酸钾加入到三口瓶中,并加入搅拌子,装上温度计,将三口瓶放入带磁力搅拌的油浴锅中,加入亚磷酸三乙酯,连接冷凝装置,开动磁力搅拌升温至120℃开始反应,反应3h,停止加热,待温度下降后,减压蒸馏,得到中间体B;
S23:将中间体A和催化剂加入到三口瓶中,再加入二甲苯溶剂和搅拌子,将三口瓶放入带磁力搅拌的油浴锅中,装上温度计、恒压漏斗,连接冷凝装置,开动磁力搅拌升温至120℃,加入中间体B,反应3h后,减压蒸馏,重结晶,过滤,得到该抗氧化剂;
步骤S2中电力管阻燃层材料的制备步骤如下:
S61:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,通入氮气,加热至120℃,电磁搅拌15h,将体系倒入到含有浓盐酸的蒸馏水中,过滤,并用蒸馏水洗涤,得到中间体C;
S62:向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,在搅拌下加热至80℃,反应8h,旋转蒸发,得到中间体D;
S63:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,通入氮气,搅拌条件下,将中间体D滴加到三口瓶中,控制滴加速度为1滴/s,加热至30℃,反应24h,倒入到含有浓盐酸的蒸馏水中,置于60℃的干燥箱真空干燥10h,得到该电力管阻燃层材料。
实施例2:
本实施例为一种具有耐热性能的MPP电力管,该具有耐热性能的MPP电力管制备方法包括如下过程:
S1:按重量份分别称取60份的聚丙烯、10份的玻璃纤维、2份的硅烷偶联剂、1份的硬脂酸、1份的石蜡和1份的抗氧化剂混合均匀,得到电力管耐热层共混料;
S2:制备电力管阻燃层材料;
S3:将S1和S2中制备的电力管耐热层共混料和电力管阻燃层材料分别加入到不同料仓干燥预热,经单螺杆挤出机挤出;
S4:采用双层共挤方式,经单螺杆挤出机挤出电力管耐热层1和电力管阻燃层2,物料由挤出机螺杆加热、熔融、塑化输送到机头口模;
S5:在单螺杆挤出机中加入重量比例为1:3的玻璃纤维和聚乙烯混合而成的中间应力层3,通过共挤的方式使电力管耐热层1和电力管阻燃层2中间形成应力层3;
步骤S1中抗氧化剂的制备步骤如下:
S21:将2,6-二叔丁基苯酚加入到装有电动搅拌器、氮气导管、温度计的三口烧瓶中,然后通入氮气吹扫,反应温度用水浴控制,将多聚甲醛和催化剂装入锥形瓶中,把锥形瓶置于磁力搅拌器上,搅拌,控制温度在50℃,待多聚甲醛完全解聚后,倒入滴液漏斗中,滴加入三口瓶中,控制滴加速度为1滴/s,反应5h,关闭氮气,充分震荡后进行减压蒸馏,重结晶,用加热套加热至其完全溶解,冷却,结晶4h后,减压抽滤,得到中间体A;
S22:将双酚B和无水碳酸钾加入到三口瓶中,并加入搅拌子,装上温度计,将三口瓶放入带磁力搅拌的油浴锅中,加入亚磷酸三乙酯,连接冷凝装置,开动磁力搅拌升温至120℃开始反应,反应3h,停止加热,待温度下降后,减压蒸馏,得到中间体B;
S23:将中间体A和催化剂加入到三口瓶中,再加入二甲苯溶剂和搅拌子,将三口瓶放入带磁力搅拌的油浴锅中,装上温度计、恒压漏斗,连接冷凝装置,开动磁力搅拌升温至120℃,加入中间体B,反应3h后,减压蒸馏,重结晶,过滤,得到该抗氧化剂;
步骤S2中电力管阻燃层材料的制备步骤如下:
S61:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,通入氮气,加热至120℃,电磁搅拌15h,将体系倒入到含有浓盐酸的蒸馏水中,过滤,并用蒸馏水洗涤,得到中间体C;
S62:向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,在搅拌下加热至80℃,反应8h,旋转蒸发,得到中间体D;
S63:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,通入氮气,搅拌条件下,将中间体D滴加到三口瓶中,控制滴加速度为2滴/s,加热至40℃,反应26h,倒入到含有浓盐酸的蒸馏水中,置于70℃的干燥箱真空干燥20h,得到该电力管阻燃层材料。
实施例3:
本实施例为一种具有耐热性能的MPP电力管,该具有耐热性能的MPP电力管制备方法包括如下过程:
S1:按重量份分别称取70份的聚丙烯、30份的玻璃纤维、4份的硅烷偶联剂、5份的硬脂酸、3份的石蜡和2份的抗氧化剂混合均匀,得到电力管耐热层共混料;
S2:制备电力管阻燃层材料;
S3:将S1和S2中制备的电力管耐热层共混料和电力管阻燃层材料分别加入到不同料仓干燥预热,经单螺杆挤出机挤出;
S4:采用双层共挤方式,经单螺杆挤出机挤出电力管耐热层1和电力管阻燃层2,物料由挤出机螺杆加热、熔融、塑化输送到机头口模;
S5:在单螺杆挤出机中加入重量比例为1:3的玻璃纤维和聚乙烯混合而成的中间应力层3,通过共挤的方式使电力管耐热层1和电力管阻燃层2中间形成应力层3;
步骤S1中抗氧化剂的制备步骤如下:
S21:将2,6-二叔丁基苯酚加入到装有电动搅拌器、氮气导管、温度计的三口烧瓶中,然后通入氮气吹扫,反应温度用水浴控制,将多聚甲醛和催化剂装入锥形瓶中,把锥形瓶置于磁力搅拌器上,搅拌,控制温度在60℃,待多聚甲醛完全解聚后,倒入滴液漏斗中,滴加入三口瓶中,控制滴加速度为2滴/s,反应6h,关闭氮气,充分震荡后进行减压蒸馏,重结晶,用加热套加热至其完全溶解,冷却,结晶8h后,减压抽滤,得到中间体A;
S22:将双酚B和无水碳酸钾加入到三口瓶中,并加入搅拌子,装上温度计,将三口瓶放入带磁力搅拌的油浴锅中,加入亚磷酸三乙酯,连接冷凝装置,开动磁力搅拌升温至130℃开始反应,反应4h,停止加热,待温度下降后,减压蒸馏,得到中间体B;
S23:将中间体A和催化剂加入到三口瓶中,再加入二甲苯溶剂和搅拌子,将三口瓶放入带磁力搅拌的油浴锅中,装上温度计、恒压漏斗,连接冷凝装置,开动磁力搅拌升温至130℃,加入中间体B,反应4h后,减压蒸馏,重结晶,过滤,得到该抗氧化剂;
步骤S2中电力管阻燃层材料的制备步骤如下:
S61:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,通入氮气,加热至130℃,电磁搅拌20h,将体系倒入到含有浓盐酸的蒸馏水中,过滤,并用蒸馏水洗涤,得到中间体C;
S62:向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,在搅拌下加热至90℃,反应10h,旋转蒸发,得到中间体D;
S63:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,通入氮气,搅拌条件下,将中间体D滴加到三口瓶中,控制滴加速度为2滴/s,加热至40℃,反应26h,倒入到含有浓盐酸的蒸馏水中,置于70℃的干燥箱真空干燥20h,得到该电力管阻燃层材料。
对比例1:
本对比例与实施例1相比未添加抗氧化剂;
对比例2:
本对比例与实施例1相比步骤S23未使用催化剂;
将实施例1-3以及对比例1-2的MPP电力管采用万能试验机,按照GB/T528-2009的标准,设定拉伸速率为500mm/min,测试材料的断裂伸长率,按照GB/T3512-2001的标准进行加速热氧老化测试,老化温度为100℃;
检测结果如下表所示:
由上表可知,在相同测试条件下,实施例的断裂伸长率达到了372-380%,而未添加抗氧化剂的对比例1的断裂伸长率为255%,而对比例2的断裂伸长率为298%,老化时间为30h的实施例的断裂伸长率保持率达到了80-82%,而老化时间为30h的未添加抗氧化剂的对比例1的断裂伸长率保持率为70%,老化时间为30h的对比例2的断裂伸长率保持率为78%,老化时间为60h的实施例的断裂伸长率保持率达到了70-75%,而老化时间为60h的未添加抗氧化剂的对比例1的断裂伸长率保持率为59%,老化时间为60h的对比例2的断裂伸长率保持率为65%,老化时间为90h的实施例的断裂伸长率保持率达到了68-72%,而老化时间为90h的未添加抗氧化剂的对比例1的断裂伸长率保持率为54%,老化时间为90h的对比例2的断裂伸长率保持率为60%,老化时间为180h的实施例的断裂伸长率保持率达到了59-62%,而老化时间为180h的未添加抗氧化剂的对比例1的断裂伸长率保持率为48%,老化时间为180h的对比例2的断裂伸长率保持率为55%,实施例的各项数据明显优于对比例,说明添加抗氧化剂明显提高了MPP电力管的抗氧化性和力学性能。
在本说明书的描述中,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 (1)
1.一种具有耐热性能的MPP电力管制备方法,包括电力管耐热层(1)、电力管阻燃层(2)和应力层(3),其特征在于,所述电力管耐热层(1)的内层设置有应力层(3),所述应力层(3)的内层设置有电力管阻燃层(2),该具有耐热性能的MPP电力管制备方法包括如下过程:
S1:按重量份分别称取60-70份的聚丙烯、10-30份的玻璃纤维、2-4份的硅烷偶联剂、1-5份的硬脂酸、1-3份的石蜡和1-2份的抗氧化剂混合均匀,得到电力管耐热层共混料;
S2:制备电力管阻燃层材料;
S3:将S1和S2中制备的电力管耐热层共混料和电力管阻燃层材料分别加入到不同料仓干燥预热,经单螺杆挤出机挤出;
S4:采用双层共挤方式,经单螺杆挤出机挤出电力管耐热层(1)和电力管阻燃层(2),物料由挤出机螺杆加热、熔融、塑化输送到机头口模;
S5:在单螺杆挤出机中加入重量比例为1:3的玻璃纤维和聚乙烯混合而成的中间应力层(3),通过共挤的方式使电力管耐热层(1)和电力管阻燃层(2)中间形成应力层(2);
步骤S1中所述抗氧化剂的制备步骤如下:
S21:将2,6-二叔丁基苯酚加入到装有电动搅拌器、氮气导管和温度计的三口烧瓶中,然后通入氮气吹扫,反应温度用水浴控制,将多聚甲醛和催化剂装入锥形瓶中,把锥形瓶置于磁力搅拌器上,搅拌,控制温度在50-60℃,待多聚甲醛完全解聚后,倒入滴液漏斗中,滴加入三口瓶中,控制滴加速度为1-2滴/s,反应5-6h,关闭氮气,充分震荡后进行减压蒸馏,重结晶,用加热套加热至其完全溶解,冷却,结晶4-8h后,减压抽滤,得到中间体A;
S22:将双酚B和无水碳酸钾加入到三口瓶中,并加入搅拌子,装上温度计,将三口瓶放入带磁力搅拌的油浴锅中,加入亚磷酸三乙酯,连接冷凝装置,开动磁力搅拌升温至120-130℃开始反应,反应3-4h,停止加热,待温度下降后,减压蒸馏,得到中间体B;
S23:将中间体A和催化剂加入到三口瓶中,再加入二甲苯溶剂和搅拌子,将三口瓶放入带磁力搅拌的油浴锅中,装上温度计和恒压漏斗,连接冷凝装置,开动磁力搅拌升温至120-130℃,加入中间体B,反应3-4h后,减压蒸馏,重结晶,过滤,得到该抗氧化剂;
步骤S2中所述电力管阻燃层材料的制备步骤如下:
S61:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺和吡啶,通入氮气,加热至120-130℃,电磁搅拌15-20h,将体系倒入到含有浓盐酸的蒸馏水中,过滤,并用蒸馏水洗涤,得到中间体C;
S62:向装有搅拌子和回流冷凝管的三颈瓶里加入中间体C和SOCl2,在搅拌下加热至80-90℃,反应8-10h,旋转蒸发,得到中间体D;
S63:向装有温度计、搅拌子、回流冷凝管和氮气进气口的三颈瓶里加入的1,4-丁炔二醇、三乙胺和N,N-二甲基乙酰胺,通入氮气,搅拌条件下,将中间体D滴加到三口瓶中,控制滴加速度为1-2滴/s,加热至30-40℃,反应24-26h,倒入到含有浓盐酸的蒸馏水中,置于60-70℃的干燥箱真空干燥10-20h,得到该电力管阻燃层材料;
步骤S21中所述催化剂为叔丁醇钾,所述2,6-二叔丁基苯酚与催化剂的用量比为4.0g:0.08g,所述2,6-二叔丁基苯酚与多聚甲醛的摩尔比为1:2.5;
步骤S22中所述双酚B与无水碳酸钾的用量比为1g:0.6g,所述双酚B与亚磷酸三乙酯的摩尔比为1:2.05;
步骤S23中所述催化剂为有机锡,所述中间体B与催化剂的用量比为0.05g:0.8g,所述中间体A与中间体B的摩尔比为4.1:1;
步骤S61中所述均苯四甲酸酐、L-苯丙氨酸、N,N-二甲基甲酰胺、吡啶、浓盐酸和蒸馏水的用量比为3.30g:5.00g:20mL:2mL:5mL:100mL;
步骤S62中所述中间体C与SOCl2的用量比为8.02g:15mL;
步骤S63中所述1,4-丁炔二醇、三乙胺、N,N-二甲基乙酰胺、中间体D、浓盐酸与蒸馏水的用量比为10.00g:3mL:20mL:8.35g:25mL:500mL。
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