CN103897243A - 一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管及其制备方法 - Google Patents

一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管及其制备方法 Download PDF

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CN103897243A
CN103897243A CN201410023049.9A CN201410023049A CN103897243A CN 103897243 A CN103897243 A CN 103897243A CN 201410023049 A CN201410023049 A CN 201410023049A CN 103897243 A CN103897243 A CN 103897243A
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徐焕辉
谢少明
李绽滨
易杜
容耀强
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CYG CHANGTONG NEW MATERIAL Co Ltd
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Abstract

本发明提供了一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管及其制备方法，首先从辐射交联聚烯烃基材的配方上突破，选择具有高机械强度和高结晶性能的高密度聚乙烯作为主料，辅以少量柔性和低温性能优异的中密度聚乙烯和加工性能良好的线性低密度聚乙烯，经配料、混料、挤出造粒、挤出片材、辐照等工序后得到热缩套管。本发明的热缩套管可以根据光缆接续盒与光缆直径的偏差实现达到的6倍率的收缩要求，又能长时间耐柴油、煤油浸泡密封不失效。

Description

一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管及其制备方法
技术领域
本发明属于材料技术领域，特别涉及一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管及其制备方法。
背景技术
热缩套管作为一种常用收缩密封材料，它是一种辐射交联聚烯烃基材和热熔胶组成，聚烯烃材料经过挤出、辐射交联、扩张后内涂覆一层特殊热熔胶，在光缆接头盒或终端盒接入光缆时，先套入光缆上，待光缆连接完成后，加热收缩热缩套管与光缆和接头盒底座导管上，使光缆与光缆接续盒光缆导管形成粘结密封，确保光缆接续盒充气压保护时，不出现漏气现象，确保外部空气、水汽无法进入，影响光缆传输效果。
目前，光缆接续盒很多时候会接触到柴油、煤油，在此环境下国内外生产的热缩套管不耐柴油、煤油，经过浸泡后，热缩套管基材和热熔胶出现溶胀等现象，造成与光缆接续盒底座连接粘结失效，光缆接续盒出现漏气，不能实现充气保护，同时目前常用热缩套管很难达到要求的6倍率的收缩要求，基本没有既能满足6倍收缩又能长时间耐柴油、煤油浸泡密封不失效的热缩套管。
所以，为了得到更高收缩要求、且满足长时间耐柴油、煤油浸泡密封不失效的热缩套管，需进一步的研究解决现有技术存在的问题。
发明内容
鉴于现有技术存在的技术问题，通过大量的实验研究发现，得到更高收缩要求，且满足长时间耐柴油、煤油浸泡密封不失效的热缩套管。
本发明通过以下技术方案解决现有技术存在的问题：
本发明目的之一在于提供一种耐柴油、煤油光缆接续密封用高收缩倍率热缩套管和其制备方法。
本发明首先从辐射交联聚烯烃基材的配方上突破，选择具有高机械强度和高结晶性能的高密度聚乙烯作为主料，辅以少量柔性和低温性能优异的中密度聚乙烯和加工性能良好的线性低密度聚乙烯，经配料、混料、挤出造粒、挤出片材、辐照等工序后得到辐射交联高密度聚乙烯基材。
本发明实现的具体方案优选为：
一种光缆接续密封用热缩套管的制备方法，包括：
基材配料→混料→挤出造粒料→挤出管坯→辐射交联→扩张
所述基材由质量比35%～50%的高密度聚乙烯（HDPE）；20%～30%的中密度聚乙烯（MDPE）；以及20%～25%的线性低密度聚乙烯（LLDPE），以及1%～2%的抗氧化剂，2%～3%的着色剂和2%～3%的加工助剂组成。
所述高密度聚乙烯的密度范围为0.941g/cm3——0.960g/cm3，所述中密度聚乙烯的密度范围为0.930g/cm3——0.939g/cm3，线性低密度聚乙烯的密度范围为0.910g/cm3——0.925g/cm3。
通过实验研究发现，本发明在配料时通过在基材中优选加入的抗氧化剂为：质量比为主抗氧剂（1010，四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯）0.5%～1%；以及质量比为辅抗氧剂（DSTDP，双硬脂酰基硫代双丙酸脂）0.5%～1%，主抗氧剂和辅抗氧剂的总量为基材质量的1%～2%的抗氧化剂。采用该质量比的主抗和辅抗混合使用，保证基材的抗热老化性能满足要求。
通过实验研究发现，本发明在配料时通过在基材中优选加入的着色剂为黑色母，采用质量比为2～3%的黑色母，可以满足热缩套管的满足着色要求，颜色光亮，以及炭黑含量满足要求。
通过实验研究发现，本发明在配料时通过在基材中优选加入的加工助剂为：质量比为2%～3%的加工助剂PPA（共聚氟化物），可以有利于管坯挤出加工，增加表面光亮度
通过大量实验研究，最优选实例为：
基材组成为：质量比为50.0%的高密度聚乙烯（密度为0.954g/cm3）；25.0%的中密度聚乙烯（密度为0.932g/cm3）；20.0%的低密度聚乙烯（密度为0.918g/cm3）；0.6%的主抗氧剂1010；0.4%的辅抗氧剂DSTDP；2.0%的黑色母；2.0%的加工助剂PPA。
通过研究发现，除了上述热缩套管的组成对其性能影响明显外，控制挤出机的工艺参数能够更好的提高热缩套管的性能，如高收缩率。
本发明的另一目的在于提供所述热缩套管的制备方法。
具体热缩套管的生产工艺（制备方法）如下：
基材配料→混料→挤出造粒料→挤出管坯→辐射交联→扩张
混料后，将均匀混合的基材原料加入双螺杆挤出机的下料口，按下列工艺挤出造粒料：
机筒：第一区：120±20℃，第二区：140±20℃，第三区：160±20℃,第四区：200±20℃，第五区：220±20℃，第六区：220±20℃，第七区：220±20℃；机头：220±20℃。
将上述工艺获得的基材造粒料经烘干后输送到单螺杆挤出机下料口，按下列工艺挤出管坯：
机筒：第一区：120±20℃，第二区：160±20℃，第三区：170±20℃,第四区：180±20℃，第五区：185±20℃，第六区：185±20℃，第七区：185±20℃；模头：190±25℃。
挤出的管坯片材规格为3.0mm～5.0mm厚，宽度根据需求裁成相应规格，挤出后的管坯经电子加速器辐射交联后扩张，扩张温度：油温170℃～190℃。
其次，本发明进一步采用以下工艺对热缩套管进行涂胶：
在耐油热熔胶的配方上，选择具有良好密封性能、粘性和耐柴油、煤油油性能复功能的多种聚酰胺材料与聚酯互配；生产工艺上采用捏合机连接挤出涂胶机，挤出涂胶机连接模具和涂胶装置，实现生产胶和涂敷胶带一次成型。
具体材料和工艺如下生产工艺如下：
胶配料为质量比为70%～85%的聚酰胺（PA，优选产品型号为163，165），10%～15%的共聚物聚酯（无规乙烯－丙烯酸酯－马来酸酐三元共聚物），0.5%～1%的色粉，0.5%～1%的抗氧剂(1010)。
胶配料→混料捏合→挤出机→涂胶→分切包装
捏合机混合温度140±15℃，捏合时间1.5～2小时熔融状态再注入螺旋涂胶机对热缩套管涂胶。
采用该配料和工艺制备的胶配料具有良好的耐煤油、耐柴油和密封性能。
相比现有技术，本发明的优点在于：
本发明热缩套管作为一种常用收缩密封材料，用于长期接触煤油、柴油等恶劣环境下光缆接续盒连接密封，确保光缆接续盒在煤油、柴油等腐蚀介质下充气压保护时，不出现漏气现象，确保外部空气、水汽无法进入，影响光缆传输效果。
本发明克服目前光缆接续盒很多时候会接触到柴油、煤油环境下国内外生产的热缩套管不耐柴油、煤油，在煤油、柴油经过浸泡120h后，热缩套管基材和热熔胶出现溶胀等现象，造成与光缆接续盒底座连接粘结失效，光缆接续盒出现漏气，不能实现充气保护，同时本发明的热缩套管可以根据光缆接续盒与光缆直径的偏差实现达到的6倍率的收缩要求，目前国内外基本没有既能满足6倍收缩又能长时间耐柴油、煤油浸泡密封不失效的热缩套管，本发明热缩套管收缩到光缆接续盒上，光缆接头盒内充气（40±2）kPa,在煤油、柴油浸泡120h后,热缩套密封部位不会发生溶胀等粘结失效，光缆接续盒内不出现漏气减压。
附图说明
图1聚乙烯基材从双螺杆挤出机造粒料的示意图
图2造粒料从单螺杆挤出机挤出管坯的示意图
具体实施方式
下面结合实施例对本发明作进一步说明：
实施例1
高密度聚乙烯（5000s，密度为0.954g/cm3）15.0%；高密度聚乙烯（C911A，密度为0.954g/cm3）35.0%；中密度聚乙烯（0588，密度为0.932g/cm3）25.0%；线性低密度聚乙烯（7042，密度为0.918g/cm3）20.0%；主抗氧剂（1010）0.6%；辅抗氧剂（DSTDP）0.4%：黑色母，2.0%，加工助剂PPA，2.0%。
基材配料→混料→挤出造粒料→挤出管坯→辐射交联→扩张
混料后，将均匀混合的基材原料加入双螺杆挤出机的下料口，按下列工艺挤出造粒料：
机筒：第一区：120±20℃，第二区：140±20℃，第三区：160±20℃,第四区：200±20℃，第五区：220±20℃，第六区：220±20℃，第七区：220±20℃；机头：220±20℃。
将上述工艺获得的基材造粒料经烘干后输送到单螺杆挤出机下料口，按下列工艺挤出管坯：
机筒：第一区：120±20℃，第二区：160±20℃，第三区：170±20℃,第四区：180±20℃，第五区：185±20℃，第六区：185±20℃，第七区：185±20℃；模头：190±25℃。
挤出的管坯片材规格为3.0厚，挤出后的管坯，经电子加速器辐射交联后扩张，扩张温度：油温170℃。
实施例2
高密度聚乙烯（5000s，密度为0.954g/cm3）25.0%；高密度聚乙烯（C911A，密度为0.954g/cm3）25.0%；中密度聚乙烯（0588，密度为0.932g/cm3）25.0%；低密度聚乙烯（FB3003，密度为0.918g/cm3）20.0%；主抗氧剂（1010）0.6%；辅抗氧剂（DSTDP）0.4%：黑色母，2.0%，加工助剂PPA，2.0%。
基材配料→混料→挤出造粒料→挤出管坯→辐射交联→扩张
混料后，将均匀混合的基材原料加入双螺杆挤出机的下料口，按下列工艺挤出造粒料：
机筒：第一区：120±20℃，第二区：140±20℃，第三区：160±20℃,第四区：200±20℃，第五区：220±20℃，第六区：220±20℃，第七区：220±20℃；机头：220±20℃。
将上述工艺获得的基材造粒料经烘干后输送到单螺杆挤出机下料口，按下列工艺挤出管坯：
机筒：第一区：120±20℃，第二区：160±20℃，第三区：170±20℃,第四区：180±20℃，第五区：185±20℃，第六区：185±20℃，第七区：185±20℃；模头：190±25℃。
挤出的管坯片材规格为3.0厚，挤出后的管坯，经电子加速器辐射交联后扩张，扩张温度：油温170℃。
实施例3热缩套管的性能检测
热熔胶涂覆在热缩套管的内表面，满足的性能要求如表1：
表1热缩套管性能要求
Figure BDA0000458300300000071
实施例1和实施例2的热缩套管均满足如表1的性能要求，且达到6倍率以上的收缩要求。
实施例4
质量比：聚酰胺PA163用65%，聚酰胺PA165用5%，聚酰胺PA20322用15%，共聚物聚酯（4210）14%；抗氧剂(1010)0.5%混合后，用加入红色粉少量（0.5%），按照下列工艺通过捏合机，混合制成胶泥：
捏合机混合温度140±15℃，捏合时间1.5～2小时熔融状态再注入螺旋涂胶机对本发明热缩套管涂胶。
实施例5
质量比：聚酰胺（PA163）75%，聚酰胺（PA20322）10%；共聚物聚酯（4210）14%；抗氧剂(1010)0.5%；红色色粉0.5%，按照下列工艺通过捏合机，混合制成胶泥：
捏合机混合温度140±15℃，捏合时间1.5～2小时熔融状态再注入螺旋涂胶机对本发明热缩套管涂胶。
实施例6涂胶热缩套管的热熔胶的性能检测
热熔胶涂覆于热缩套管的内表面，满足的性能要求如表2：
表2热熔胶性能要求
Figure BDA0000458300300000081
实施例4和实施例5涂覆了热熔胶的热缩套管均满足如表2的性能要求，能长时间耐柴油、煤油浸泡密封不失效，本发明热缩套管收缩到光缆接续盒上，光缆接头盒内充气（40±2）kPa,在煤油、柴油浸泡120h后,热缩套密封部位不会发生溶胀等粘结失效，光缆接续盒内不出现漏气减压。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。

Claims (10)

1.一种光缆接续密封用热缩套管的制备方法，包括：
基材配料→混料→挤出造粒料→挤出管坯→辐射交联→扩张
所述基材由质量比35%～50%的高密度聚乙烯（HDPE）；20%～30%的中密度聚乙烯（MDPE）；以及20%～25%的线性低密度聚乙烯（LLDPE），以及1%～2%的抗氧化剂，2%～3%的着色剂和2%～3%的加工助剂组成。
2.根据权利要求1所述的制备方法，其特征在于，所述高密度聚乙烯的密度范围为0.941g/cm3——0.960g/cm3，所述中密度聚乙烯的密度范围为0.930g/cm3——0.939g/cm3，线性低密度聚乙烯的密度范围为0.910g/cm3——0.925g/cm3。
3.根据权利要求1所述的制备方法，其特征在于，在配料时加入的抗氧化剂由主抗氧剂和辅抗氧剂组成，其中，为质量比0.5%～1%主抗氧剂四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯；以及质量比0.5%～1%的辅抗氧剂双硬脂酰基硫代双丙酸脂。
4.根据权利要求1所述的制备方法，其特征在于，在配料时加入的着色剂为黑色母，加工助剂为PPA。
5.根据权利要求1所述的制备方法，其特征在于，基材组成为质量比为50.0%的高密度聚乙烯（密度为0.954g/cm3）；25.0%的中密度聚乙烯（密度为0.932g/cm3）；20.0%的低密度聚乙烯（密度为0.918g/cm3）；0.6%的主抗氧剂1010；0.4%的辅抗氧剂DSTDP；2.0%的黑色母；2.0%的加工助剂PPA。
6.根据权利要求1—5任一权利要求所述的制备方法，其特征在于，混料后，将均匀混合的基材原料加入双螺杆挤出机的下料口，按下列工艺挤出造粒料：
机筒：第一区：120±20℃，第二区：140±20℃，第三区：160±20℃,第四区：200±20℃，第五区：220±20℃，第六区：220±20℃，第七区：220±20℃；机头：220±20℃。
将上述工艺获得的基材造粒料经烘干后输送到单螺杆挤出机下料口，按下列工艺挤出管坯：
机筒：第一区：120±20℃，第二区：160±20℃，第三区：170±20℃,第四区：180±20℃，第五区：185±20℃，第六区：185±20℃，第七区：185±20℃；模头：190±25℃。
挤出的管坯片材规格为3.0mm～5.0mm厚，挤出后的管坯，经电子加速器辐射交联后扩张，扩张温度：油温170℃～190℃。
7.根据权利要求1—5任一权利要求所述的制备方法，其特征在于，进一步采用胶配料对热缩套管内部进行涂胶，所述工艺为：胶配料→混料捏合→挤出机→涂胶→分切包装。
8.根据权利要求7所述的制备方法，其特征在于，胶配料为质量比为70%～85%的聚酰胺，10%～15%的共聚物聚酯(无规乙烯－丙烯酸酯－马来酸酐三元共聚物)，0.5%～1%的色粉，0.5%～1%的抗氧剂四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯。
9.根据权利要求7所述的制备方法，其特征在于，所述混料捏合的工艺为捏合机混合温度140±15℃，捏合时间1.5～2小时熔融状态再注入螺旋涂胶机对热缩套管涂胶。
10.根据权利要求8所述的制备方法，其特征在于，所述混料捏合的工艺为捏合机混合温度140±15℃，捏合时间1.5～2小时熔融状态再注入螺旋涂胶机对热缩套管涂胶。
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