CN116462896A - 一种低烟无卤阻燃光缆用护套料及其制备方法 - Google Patents
一种低烟无卤阻燃光缆用护套料及其制备方法 Download PDFInfo
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- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract
本发明公开了一种低烟无卤阻燃光缆用护套料及其制备方法,属于光缆护套技术领域,包括以下原料聚乙烯树脂、聚丙烯树脂、填料、增塑剂、阻燃剂、复合稳定剂、抗氧剂、润滑剂和相容剂;复合稳定剂包括改性膨胀石墨、2‑氨基‑5‑吡啶羧酸镧和4,4'‑二羟基二苯甲酮镧,2‑氨基‑5‑吡啶羧酸镧和4,4'‑二羟基二苯甲酮镧能够防止氯化氢气体对护套料的催化降解,增加护套料的热稳定性;改性石墨经过聚乙烯吡咯烷酮修饰后有助于提升分散性,在较高温度条件下不仅起到阻燃作用,还可以吸收产生的氯化氢气体,配合2‑氨基‑5‑吡啶羧酸镧和4,4'‑二羟基二苯甲酮镧协同处理氯化氢。
Description
技术领域
本发明属于光缆护套技术领域,具体涉及一种低烟无卤阻燃光缆用护套料及其制备方法。
背景技术
光缆是一种为了满足光学、机械或环境的性能规范而制造的线缆,它是利用置于包覆护套中的一根或多根光纤作为传输媒质并可以单独或成组使用的通信线缆组件,光缆的基本结构一般是由缆芯、加强钢丝、填充物和护套等几部分组成,另外根据需要还有防水层、缓冲层、绝缘金属导线等构件。
为了便于光缆铺设和运输,一般新出厂的光缆每轴可卷2千到3千米,在长距离铺设光缆时需要将不同轴的光缆进行接续,接续时两轴光缆在护套内进行接续。一般光缆护套包括聚乙烯护套、金属粘接护套和53型护套,其中聚乙烯护套加工工艺简单,成本低,常用于普通敷设场合,缆芯直接与护套紧密接触,防水性能不如其他护套;金属粘接护套利用复合钢带或铝带在塑料挤出过程中与塑料粘结形成一个完整的整体。粘结护层的优点是能经受各种热应力时,护套具有抗尺寸变化的特性,这种特性是由于护套结构的金属元件和塑料组成一个整体,使其具有两种元件的最佳特性。护套树脂粘结到了金属带上,所有塑料的热膨胀系数就由所依附的金属带的热膨胀系数决定,因此粘结护层结构几乎不发生收缩;53型护套结构主要由内护层、铠装层和外护层组成;内护层的主要作用是在铠装过程中作为铠装层的衬垫,可以防止缆芯被铠装层压伤,还可以在敷设运行中抵御外界腐浊介质的侵入,防止金属护套与外界腐蚀介质接触。
光缆作为现代通讯的支柱之一,在物联网、大数据、虚拟现实、人工智能和第五代移动通信等技术领域应用广泛,面对复杂的应用环境,为了保证光缆使用的稳定性,防止光缆护套材料老化对光缆使用寿命产生影响,因此提出一种低烟无卤阻燃光缆用护套料及其制备方法。
发明内容
本发明的目的在于提供一种低烟无卤阻燃光缆用护套料及其制备方法,以解决背景技术中的问题。
本发明的目的可以通过以下技术方案实现:
一种低烟无卤阻燃光缆用护套料,按质量份计包括如下组分:
该低烟无卤阻燃光缆用护套料通过如下步骤制备:
步骤一:将聚乙烯树脂、聚丙烯树脂、填料和改性剂在60℃条件下真空干燥12h。
步骤二:将聚乙烯树脂、聚丙烯树脂、填料、增塑剂、阻燃剂、复合稳定剂、抗氧剂润滑剂和相容剂在200-300r/min的条件下搅拌5-10min,然后投入密炼机中在140-160℃的条件下密炼15-30min,将密炼后的物料转移至双螺杆挤出机中,在150℃的条件下挤出,造粒,得到低烟无卤阻燃光缆用护套料。
进一步地,填料为白炭黑。
进一步地,增塑剂为邻苯二甲酸二辛酯和对苯二甲酸二辛酯中的一种或两种按任意比混合。
进一步地,阻燃剂为氢氧化镁和氢氧化铝中的任意一种。
进一步地,抗氧剂为抗氧剂1010或抗氧剂168。
进一步地,润滑剂为硬脂酸。
进一步地,相容剂为改性聚乙烯树脂。
进一步地,复合稳定剂通过如下步骤制备:
步骤1:将硝酸镧用无水乙醇搅拌溶解,得到质量浓度为350g/L的硝酸镧溶液。
步骤2:将2-氨基-5-吡啶羧酸和氢氧化钠加入烧瓶中,然后向烧瓶中加入去离子水并搅拌15-20min,得到2-氨基-5-吡啶羧酸分散液,将2-氨基-5-吡啶羧酸分散液在85-90℃的条件下搅拌15-30min,然后滴加硝酸镧溶液,用氢氧化钠溶液调节pH值至6.5±0.2,继续搅拌2-3h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤3-5次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到2-氨基-5-吡啶羧酸镧;
2-氨基-5-吡啶羧酸、氢氧化钠、去离子水和硝酸镧溶液的用量比为4.2g:0.4g:20-30mL:28mL。
步骤3:将4,4'-二羟基二苯甲酮用无水乙醇搅拌溶解,然后向其中滴加硝酸镧溶液并搅拌30-45min,然后用氢氧化钠溶液调节pH值至6±0.2,继续搅拌3-4h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤3-5次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到4,4'-二羟基二苯甲酮镧;
4,4'-二羟基二苯甲酮、无水乙醇和硝酸镧溶液的用量比为6.5g:50mL:8mL。
步骤4:将聚乙烯吡咯烷酮用去离子水溶解,然后加入膨胀石墨,在800-1000r/min的条件下搅拌6-10h,然后减压抽滤,得到改性膨胀石墨;将改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:1:1-2的质量比混合球磨混合,过滤出料得到复合稳定剂。
本发明的有益效果:
本发明低烟无卤阻燃光缆用护套料通过无卤阻燃剂达到低烟无卤阻燃效果,并且添加复合稳定剂后具有较好的热稳定和光稳定效果。其中聚丙烯树脂可以提高材料内部无机粒子与聚合物基体之间的相互作用,保证该护套料性能的均一性,提高线缆材料热稳定和阻燃性能,保证生产出的光缆护套的强度。
本发明中复合稳定剂包括改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧,2-氨基-5-吡啶羧酸和4,4'-二羟基二苯甲酮具有紫外光吸收作用,有助于增加材料的光稳定性。2-氨基-5-吡啶羧酸和4,4'-二羟基二苯甲酮分别与硝酸镧发生复分解反应制备出2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧,其中含有氨基和不饱和双键,通过加成反应吸收光缆护套料产生的氯化氢气体,镧元素也可以生产氯化物从而减少氯化氢的含量,从而防止氯化氢气体对护套料的催化降解,增加护套料的热稳定性。改性石墨经过聚乙烯吡咯烷酮修饰后有助于提升分散性,在较高温度条件下不仅起到阻燃作用,还可以吸收产生的氯化氢气体,配合2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧协同处理氯化氢。
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
本实施制备复合稳定剂,包括如下实施步骤:
步骤1:将硝酸镧用无水乙醇搅拌溶解,得到质量浓度为350g/L的硝酸镧溶液。
步骤2:将42g 2-氨基-5-吡啶羧酸和4g氢氧化钠加入烧瓶中,然后向烧瓶中加入200mL去离子水并搅拌15min,得到2-氨基-5-吡啶羧酸分散液,将2-氨基-5-吡啶羧酸分散液在85-90℃的条件下搅拌15min,然后滴加28mL硝酸镧溶液,用氢氧化钠溶液调节pH值至6.5±0.2,继续搅拌2h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤3次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到2-氨基-5-吡啶羧酸镧。
步骤3:将65g 4,4'-二羟基二苯甲酮用500mL无水乙醇搅拌溶解,然后向其中滴加80mL硝酸镧溶液并搅拌30min,然后用氢氧化钠溶液调节pH值至6±0.2,继续搅拌3-4h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤3次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到4,4'-二羟基二苯甲酮镧。
步骤4:将聚乙烯吡咯烷酮用去离子水溶解,然后加入膨胀石墨,在800r/min的条件下搅拌6h,然后减压抽滤,得到改性膨胀石墨;将改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:1:1的质量比混合球磨混合,过滤出料得到复合稳定剂。
实施例2
本实施制备复合稳定剂,包括如下实施步骤:
步骤1:将硝酸镧用无水乙醇搅拌溶解,得到质量浓度为350g/L的硝酸镧溶液。
步骤2:将42g 2-氨基-5-吡啶羧酸和4g氢氧化钠加入烧瓶中,然后向烧瓶中加入250mL去离子水并搅拌18min,得到2-氨基-5-吡啶羧酸分散液,将2-氨基-5-吡啶羧酸分散液在88℃的条件下搅拌20min,然后滴加28mL硝酸镧溶液,用氢氧化钠溶液调节pH值至6.5±0.2,继续搅拌2.5h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤4次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到2-氨基-5-吡啶羧酸镧。
步骤3:将65g 4,4'-二羟基二苯甲酮用500mL无水乙醇搅拌溶解,然后向其中滴加80mL硝酸镧溶液并搅拌40min,然后用氢氧化钠溶液调节pH值至6±0.2,继续搅拌3.5h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤4次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到4,4'-二羟基二苯甲酮镧。
步骤4:将聚乙烯吡咯烷酮用去离子水溶解,然后加入膨胀石墨,在900r/min的条件下搅拌8h,然后减压抽滤,得到改性膨胀石墨;将改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:1:1.5的质量比混合球磨混合,过滤出料得到复合稳定剂。
实施例3
本实施制备复合稳定剂,包括如下实施步骤:
步骤1:将硝酸镧用无水乙醇搅拌溶解,得到质量浓度为350g/L的硝酸镧溶液。
步骤2:将42g 2-氨基-5-吡啶羧酸和4g氢氧化钠加入烧瓶中,然后向烧瓶中加入300mL去离子水并搅拌20min,得到2-氨基-5-吡啶羧酸分散液,将2-氨基-5-吡啶羧酸分散液在90℃的条件下搅拌30min,然后滴加28mL硝酸镧溶液,用氢氧化钠溶液调节pH值至6.5±0.2,继续搅拌3h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤3-5次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到2-氨基-5-吡啶羧酸镧。
步骤3:将65g 4,4'-二羟基二苯甲酮用500mL无水乙醇搅拌溶解,然后向其中滴加80mL硝酸镧溶液并搅拌45min,然后用氢氧化钠溶液调节pH值至6±0.2,继续搅拌3-4h,冷却并生成沉淀后减压抽滤,将滤饼用无水乙醇洗涤5次,然后置于真空干燥箱中在60℃的条件下干燥至恒重,得到4,4'-二羟基二苯甲酮镧。
步骤4:将聚乙烯吡咯烷酮用去离子水溶解,然后加入膨胀石墨,在1000r/min的条件下搅拌10h,然后减压抽滤,得到改性膨胀石墨;将改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:1:2的质量比混合球磨混合,过滤出料得到复合稳定剂。
实施例4
本实施例制备低烟无卤阻燃光缆用护套料,包括如下实施步骤:
步骤一:将聚乙烯树脂、聚丙烯树脂、填料和改性剂在60℃条件下真空干燥12h。
步骤二:将10kg聚乙烯树脂、1-1.5kg聚丙烯树脂、1-2kg白炭黑、1kg按1:1质量比混合的邻苯二甲酸二辛酯和对苯二甲酸二辛酯、1kg氢氧化镁、0.5kg实施例1中制备的复合稳定剂、10g抗氧剂1010、0.1kg硬脂酸和2kg改性聚乙烯树脂在200r/min的条件下搅拌5min,然后投入密炼机中在140℃的条件下密炼15min,将密炼后的物料转移至双螺杆挤出机中,在150℃的条件下挤出,造粒,得到低烟无卤阻燃光缆用护套料。
实施例5
本实施例制备低烟无卤阻燃光缆用护套料,包括如下实施步骤:
步骤一:将聚乙烯树脂、聚丙烯树脂、填料和改性剂在60℃条件下真空干燥12h。
步骤二:将10kg聚乙烯树脂、1.2kg聚丙烯树脂、1.5kg白炭黑、2kg邻苯二甲酸二辛酯、1.5kg氢氧化镁、0.6kg实施例2中制备的复合稳定剂、15g抗氧剂1010、0.2kg硬脂酸和2.5kg改性聚乙烯树脂在250r/min的条件下搅拌8min,然后投入密炼机中在150℃的条件下密炼20min,将密炼后的物料转移至双螺杆挤出机中,在150℃的条件下挤出,造粒,得到低烟无卤阻燃光缆用护套料。
实施例6
本实施例制备低烟无卤阻燃光缆用护套料,包括如下实施步骤:
步骤一:将聚乙烯树脂、聚丙烯树脂、填料和改性剂在60℃条件下真空干燥12h。
步骤二:将10kg聚乙烯树脂、1.5kg聚丙烯树脂、2kg白炭黑、1-3kg对苯二甲酸二辛酯、2kg氢氧化铝、0.8kg实施例3中制备的复合稳定剂、20g抗氧剂168、0.3kg硬脂酸和3kg改性聚乙烯树脂在300r/min的条件下搅拌10min,然后投入密炼机中在160℃的条件下密炼30min,将密炼后的物料转移至双螺杆挤出机中,在150℃的条件下挤出,造粒,得到低烟无卤阻燃光缆用护套料。
对比例1:在实施例3的基础上,不添加改性膨胀石墨,直接将2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:2的质量比混合球磨混合,制备出复合稳定剂,然后按照实施例6的方法并替代其中的复合稳定剂,其余步骤保持不变,制备出护套料。
对比例2:在实施例3的基础上,不添加2-氨基-5-吡啶羧酸镧,直接将改性膨胀石墨和4,4'-二羟基二苯甲酮镧按照1:2质量比混合球磨混合,制备出复合稳定剂,然后按照实施例6的方法并替代其中的复合稳定剂,其余步骤保持不变,制备出护套料。
对比例3:在实施例6的基础上,不添加复合稳定剂,其余步骤保持不变,制备出护套料。
上述白炭黑购买于石家庄市勤迈化工科技有限公司;膨胀石墨购买于灵寿县石峰矿业,2000目;改性聚乙烯树脂购买于宁波能之光新材料科技有限公司,牌号为MC218;聚乙烯树脂牌号为SG-5;聚丙烯树脂为日本三井化学生产,牌号为260。
对实施例4-实施例6和对比例1-对比例3进行性能测试,根据ISO182-1中的刚果红试验,将6组制备出的护套料研磨粉碎得到六组样品,然后将不同样品分别装入15mL试管中,在样品上方2cm处放上润湿的刚果红试纸,在180℃油浴的条件下测试,记录刚果红试纸变蓝所需时间;然后在300℃油浴的条件下再次测试刚果红试纸变蓝所需时间。根据GB/T1040-2006将对实施例4-实施例6和对比例1-对比例3中的护套料分别制备出六组试样(每组试样制备5个样片,长150mm,宽10mm,厚3mm),然后按照GB/T 3681-2011将不同样片在自然条件下暴露40天,每隔10天测试一次力学性能(测试地点:苏州市,平均气温26℃,平均相对湿度58%)。结果如表1所示:
表1
由表1可以看出,实施例4-实施例6中低烟无卤阻燃光缆用护套料具有较好的热稳定性和光稳定性,在300℃条件下,含有改性膨胀石墨的热稳定效果更好,是因为膨胀石墨在290℃条件下开始膨胀,有助于吸收氯化氢气体有利于复合稳定剂中其余组分吸收固定氯。
需要说明的是,在本文中,诸如术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种低烟无卤阻燃光缆用护套料,其特征在于,按质量份计,包括以下原料:
聚乙烯树脂100份、聚丙烯树脂10-15份、填料10-20份、增塑剂10-30份、阻燃剂10-20份、复合稳定剂5-8份、抗氧剂0.1-0.2份、润滑剂1-3份和相容剂20-30份;
所述复合稳定剂通过如下步骤制备:
将聚乙烯吡咯烷酮用去离子水溶解,加入膨胀石墨在800-1000r/min的条件下搅拌6-10h,减压抽滤,得到改性膨胀石墨;将改性膨胀石墨、2-氨基-5-吡啶羧酸镧和4,4'-二羟基二苯甲酮镧按照1:1:1-2的质量比混合球磨混合,过滤出料得到复合稳定剂。
2.根据权利要求1所述的一种低烟无卤阻燃光缆用护套料,其特征在于,所述2-氨基-5-吡啶羧酸镧通过如下步骤制备:
将2-氨基-5-吡啶羧酸、氢氧化钠用去离子水并搅拌混合,得到2-氨基-5-吡啶羧酸分散液,然后在85-90℃的条件下搅拌15-30min,滴加硝酸镧溶液,用氢氧化钠溶液调节pH值至6.5±0.2,继续搅拌2-3h,冷却,减压抽滤,洗涤滤饼并干燥,得到2-氨基-5-吡啶羧酸镧。
3.根据权利要求2所述的一种低烟无卤阻燃光缆用护套料,其特征在于,所述2-氨基-5-吡啶羧酸、氢氧化钠、去离子水和硝酸镧溶液的用量比为4.2g:0.4g:20-30mL:28mL。
4.根据权利要求1所述的一种低烟无卤阻燃光缆用护套料,其特征在于,所述4,4'-二羟基二苯甲酮镧通过如下步骤制备:
将4,4'-二羟基二苯甲酮用无水乙醇搅拌溶解,加入硝酸镧溶液并搅拌30-45min,然后用氢氧化钠溶液调节pH值至6±0.2,继续搅拌3-4h,冷却,减压抽滤,将滤饼洗涤,干燥,得到4,4'-二羟基二苯甲酮镧。
5.根据权利要求4所述的一种低烟无卤阻燃光缆用护套料,其特征在于,所述4,4'-二羟基二苯甲酮、无水乙醇和硝酸镧溶液的用量比为6.5g:50mL:8mL。
6.根据权利要求3或5所述的一种低烟无卤阻燃光缆用护套料,其特征在于,所述硝酸镧溶液的质量浓度为350g/L。
7.根据权利要求1所述的一种低烟无卤阻燃光缆用护套料的制备方法,其特征在于,包括如下步骤:
步骤一:将聚乙烯树脂、聚丙烯树脂、填料和改性剂在60℃条件下真空干燥12h;
步骤二:将聚乙烯树脂、聚丙烯树脂、填料、增塑剂、阻燃剂、复合稳定剂、抗氧剂润滑剂和相容剂在200-300r/min的条件下搅拌5-10min,然后投入密炼机中在140-160℃的条件下密炼15-30min,将密炼后的物料转移至双螺杆挤出机中,在150℃的条件下挤出,造粒,得到低烟无卤阻燃光缆用护套料。
8.根据权利要求7所述的一种低烟无卤阻燃光缆用护套料的制备方法,其特征在于,所述增塑剂为邻苯二甲酸二辛酯和对苯二甲酸二辛酯中的一种或两种按任意比混合。
9.根据权利要求7所述的一种低烟无卤阻燃光缆用护套料的制备方法,其特征在于,阻燃剂为氢氧化镁和氢氧化铝中的任意一种。
10.根据权利要求7所述的一种低烟无卤阻燃光缆用护套料的制备方法,其特征在于,所述抗氧剂为抗氧剂1010或抗氧剂168。
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