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Article(id=1209927477208675238, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927476046860302, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2022.05.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1626105600000, receivedDateStr=2021-07-13, revisedDate=1631376000000, revisedDateStr=2021-09-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1766398789932, onlineDateStr=2025-12-22, pubDate=1652976000000, pubDateStr=2022-05-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766398789932, onlineIssueDateStr=2025-12-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766398789932, creator=13701087609, updateTime=1766398789932, updator=13701087609, issue=Issue{id=1209927476046860302, tenantId=1146029695717560320, journalId=1149653034449285133, year='2022', volume='55', issue='5', pageStart='1', pageEnd='122', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766398789655, creator=13701087609, updateTime=1766563075277, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210616539955466501, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927476046860302, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210616539959660806, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1209927476046860302, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=35, endPage=41, ext={EN=ArticleExt(id=1209927477430973351, articleId=1209927477208675238, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Properties of Polypropylene Based Insulating Materials Improved by Grafting Voltage Stabilizer, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

The aromatic ketone polymer 4-allyloxy-2-hydroxybenzophenone (AOHBP) was selected as voltage stabilizer. In order to inhibit the migration and precipitation of voltage stabilizer in polymer, dicumyl peroxide (DCP) was used as initiator to graft AOHBP on PP, and an anti-degradation additive styrene derivative (St) was added to inhibit the material degradation caused by the grafting process of voltage stabilizer. The physical and chemical properties of the modified material were characterized, and the electrical treeing initiation characteristics and DC breakdown characteristics of the modified material were studied. The results show that the AOHBP can graft on the PP matrix by the free radical reaction initiated by DCP, and the St and AOHBP can inhibit the macromolecular degradation of PP during the grafting reaction process synergistically. The grafting modified PP insulating material can inhibit the initiation of electrical tree and improve the DC electric strength significantly.

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选取芳香酮类聚合物4-丙烯氧基-2-羟基二苯甲酮（AOHBP）为电压稳定剂，同时为了抑制其在聚合物中的迁移和析出，采用过氧化二异丙苯（DCP）作为接枝反应引发剂，将AOHBP接枝在PP上，并加入防降解添加剂苯乙烯衍生物（St）来抑制电压稳定剂接枝过程导致的材料降解，然后对改性材料的理化特性进行表征，最后对改性材料电树枝的引发特性和直流击穿特性进行了研究。结果表明：AOHBP可以通过DCP引发的自由基反应接枝在PP基体上，且St和AOHBP可以共同抑制接枝反应过程中PP的大分子降解；接枝改性PP绝缘材料可显著抑制电树枝的引发并提高其直流电气强度。

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李春阳（1991-），男（汉族），黑龙江哈尔滨人，讲师，研究方向为高压电力电缆及其附件用聚合物绝缘材料。
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邵满智（1997-），男（汉族），内蒙古锡林郭勒盟人，硕士生，研究方向为电缆聚合物绝缘材料。

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邵满智（1997-），男（汉族），内蒙古锡林郭勒盟人，硕士生，研究方向为电缆聚合物绝缘材料。

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邵满智（1997-），男（汉族），内蒙古锡林郭勒盟人，硕士生，研究方向为电缆聚合物绝缘材料。

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试样PPAOHBPDCPSt
PP100000
PP+0.2DCP10000.20
PP+1St+0.2DCP10000.21
PP+1St+0.6AOHBP1000.601
PP+1St+0.6AOHBP+0.2DCP1000.60.21
), ArticleFig(id=1210884597324321050, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=CN, label=表1, caption=

材料配方

, figureFileSmall=null, figureFileBig=null, tableContent=
试样PPAOHBPDCPSt
PP100000
PP+0.2DCP10000.20
PP+1St+0.2DCP10000.21
PP+1St+0.6AOHBP1000.601
PP+1St+0.6AOHBP+0.2DCP1000.60.21
), ArticleFig(id=1210884597429178654, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=EN, label=Tab.2, caption=Melt index test results, figureFileSmall=null, figureFileBig=null, tableContent=
试样熔融指数/(g/10min)
PP4.2
PP+0.2DCP28.0
PP+1St+0.2DCP11.1
PP+1St+0.6AOHBP+0.2DCP7.3
), ArticleFig(id=1210884597521453346, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=CN, label=表2, caption=

熔融指数测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样熔融指数/(g/10min)
PP4.2
PP+0.2DCP28.0
PP+1St+0.2DCP11.1
PP+1St+0.6AOHBP+0.2DCP7.3
), ArticleFig(id=1210884597622116646, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=EN, label=Tab.3, caption=Tensile test results of each PP sample, figureFileSmall=null, figureFileBig=null, tableContent=
试样断裂伸长率/%拉伸断裂应力/MPa拉伸屈服应力/MPa
PP415.216.214.8
PP+0.2DCP36.311.110.8
PP+1St+0.2DCP312.213.311.0
PP+1St+0.6AOHBP+0.2DCP488.721.016.9
), ArticleFig(id=1210884597718585640, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=CN, label=表3, caption=

各PP试样拉伸测试结果

, figureFileSmall=null, figureFileBig=null, tableContent=
试样断裂伸长率/%拉伸断裂应力/MPa拉伸屈服应力/MPa
PP415.216.214.8
PP+0.2DCP36.311.110.8
PP+1St+0.2DCP312.213.311.0
PP+1St+0.6AOHBP+0.2DCP488.721.016.9
), ArticleFig(id=1210884597848609068, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=EN, label=Tab.4, caption=DSC crystallization parameters of each PP sample, figureFileSmall=null, figureFileBig=null, tableContent=
参数PPPP+0.2DCPPP+1St+0.2DCPPP+1St+0.6AOHBP+0.2DCP
结晶度/%43.739.240.039.6
熔融峰温度/℃166.5165.4162.7164.5
结晶峰温度/℃121.4120.6120.1121.4
), ArticleFig(id=1210884597940883760, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=CN, label=表4, caption=

各PP试样的DSC结晶参数

, figureFileSmall=null, figureFileBig=null, tableContent=
参数PPPP+0.2DCPPP+1St+0.2DCPPP+1St+0.6AOHBP+0.2DCP
结晶度/%43.739.240.039.6
熔融峰温度/℃166.5165.4162.7164.5
结晶峰温度/℃121.4120.6120.1121.4
), ArticleFig(id=1210884598054129972, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=EN, label=Tab.5, caption=Initiation voltage and extinction voltage of electrical tree partial discharge for each sample, figureFileSmall=null, figureFileBig=null, tableContent=
试样起始电压/kV熄灭电压/kV
PP7.63.3
PP+0.6AOHBP10.14.4
PP+1St+0.6AOHBP7.53.1
PP+0.6AOHPB+0.2DCP7.33.0
PP+1St+0.2DCP7.53.1
PP+1St+0.6AOHBP+0.2DCP9.53.9
), ArticleFig(id=1210884598142210361, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1209927477208675238, language=CN, label=表5, caption=

各试样的电树枝起始电压与熄灭电压

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试样起始电压/kV熄灭电压/kV
PP7.63.3
PP+0.6AOHBP10.14.4
PP+1St+0.6AOHBP7.53.1
PP+0.6AOHPB+0.2DCP7.33.0
PP+1St+0.2DCP7.53.1
PP+1St+0.6AOHBP+0.2DCP9.53.9
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电压稳定剂接枝改善聚丙烯基绝缘材料性能研究
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邵满智 1 , 万玉鑫 1 , 牛越 2 , 李春阳 1 , 赵洪 1 , 岳振国 3
绝缘材料 | 材料研究 2022,55(5): 35-41
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绝缘材料 | 材料研究 2022, 55(5): 35-41
电压稳定剂接枝改善聚丙烯基绝缘材料性能研究
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邵满智1, 万玉鑫1, 牛越2, 李春阳1, 赵洪1, 岳振国3
作者信息
  • 1哈尔滨理工大学 工程电介质及其应用技术教育部重点实验室,黑龙江 哈尔滨 150080
  • 2国网内蒙古东部电力有限公司赤峰供电公司,内蒙古 赤峰 024000
  • 3浙江晨光电缆股份有限公司,浙江 平湖 314204

    • 邵满智（1997-），男（汉族），内蒙古锡林郭勒盟人，硕士生，研究方向为电缆聚合物绝缘材料。

通讯作者:

李春阳（1991-），男（汉族），黑龙江哈尔滨人，讲师，研究方向为高压电力电缆及其附件用聚合物绝缘材料。
Properties of Polypropylene Based Insulating Materials Improved by Grafting Voltage Stabilizer
Manzhi SHAO1, Yuxin WAN1, Yue NIU2, Chunyang LI1, Hong ZHAO1, Zhenguo YUE3
Affiliations
  • 1Key Laboratory of Engineering Dielectrics and Its Application, Ministry of Education, Harbin University of Science and Technology, Harbin 150080, China
  • 2Chifeng Power Supply Company, State Grid East Inner Mongolia Electric Power Company Limited, Chifeng 024000, China
  • 3Zhejiang Chenguang Cable Company Limited, Pinghu 314204, China
出版时间: 2022-05-20 doi: 10.16790/j.cnki.1009-9239.im.2022.05.005
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摘要
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选取芳香酮类聚合物4-丙烯氧基-2-羟基二苯甲酮（AOHBP）为电压稳定剂，同时为了抑制其在聚合物中的迁移和析出，采用过氧化二异丙苯（DCP）作为接枝反应引发剂，将AOHBP接枝在PP上，并加入防降解添加剂苯乙烯衍生物（St）来抑制电压稳定剂接枝过程导致的材料降解，然后对改性材料的理化特性进行表征，最后对改性材料电树枝的引发特性和直流击穿特性进行了研究。结果表明：AOHBP可以通过DCP引发的自由基反应接枝在PP基体上，且St和AOHBP可以共同抑制接枝反应过程中PP的大分子降解；接枝改性PP绝缘材料可显著抑制电树枝的引发并提高其直流电气强度。

聚丙烯  /  电压稳定剂  /  电树枝  /  直流击穿

The aromatic ketone polymer 4-allyloxy-2-hydroxybenzophenone (AOHBP) was selected as voltage stabilizer. In order to inhibit the migration and precipitation of voltage stabilizer in polymer, dicumyl peroxide (DCP) was used as initiator to graft AOHBP on PP, and an anti-degradation additive styrene derivative (St) was added to inhibit the material degradation caused by the grafting process of voltage stabilizer. The physical and chemical properties of the modified material were characterized, and the electrical treeing initiation characteristics and DC breakdown characteristics of the modified material were studied. The results show that the AOHBP can graft on the PP matrix by the free radical reaction initiated by DCP, and the St and AOHBP can inhibit the macromolecular degradation of PP during the grafting reaction process synergistically. The grafting modified PP insulating material can inhibit the initiation of electrical tree and improve the DC electric strength significantly.

polypropylene  /  voltage stabilizer  /  electrical tree  /  DC breakdown
邵满智, 万玉鑫, 牛越, 李春阳, 赵洪, 岳振国. 电压稳定剂接枝改善聚丙烯基绝缘材料性能研究. 绝缘材料, 2022 , 55 (5) : 35 -41 . DOI: 10.16790/j.cnki.1009-9239.im.2022.05.005
Manzhi SHAO, Yuxin WAN, Yue NIU, Chunyang LI, Hong ZHAO, Zhenguo YUE. Properties of Polypropylene Based Insulating Materials Improved by Grafting Voltage Stabilizer[J]. Insulating Materials, 2022 , 55 (5) : 35 -41 . DOI: 10.16790/j.cnki.1009-9239.im.2022.05.005
正文
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0 引言
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随着我国城市化进程的不断推进，电力电缆用量以及人们对于电力电缆运行稳定性的要求逐年提高。目前，具有较好电气性能和力学性能的材料——交联聚乙烯（XLPE）是电力电缆的主要绝缘介质，但是XLPE为热固性材料，当电缆达到运行年限后便不可回收利用，只能焚烧填埋，造成极大的资源浪费。相比之下，聚丙烯（PP）绝缘材料熔点高、电气性能优异，无需交联即可具有较高的机械强度和耐高温性能，且作为热塑性材料可以回收再利用，符合未来大容量、环境友好型电缆的发展需求[1-2]。因此，未来采用PP代替XLPE作为电力电缆绝缘将带来极大的经济效益和社会效益，符合绿色环保的发展理念和价值取向，无论应用于交流电缆还是直流电缆，都具备很大的发展潜力[3]。
I L HOSIER等[4]使用一种金属茂络合物催化剂制备了一种新型间规聚丙烯（s-PP）。研究表明，采用s-PP作为主绝缘的电缆表现出与传统的等规聚丙烯（i-PP）不同的特性，除了克服其弹性差、易形成球状结构和易降解的缺点外，s-PP还表现出良好的电气性能。D W KIM等[5]也对s-PP和i-PP的分子结构和电气性能等进行比较。结果发现，s-PP在高温下形成的球晶粒径为i-PP的1/30～1/20，因此s-PP具有更好的电气性能和热稳定性，但因其价格较高，难以大量投入使用。G PEREGO等[6]通过接枝马来酸酐对PP进行材料改性。研究发现，接枝马来酸酐后PP的电气性能提高，主要表现为电气强度提高，空间电荷积聚量下降。其原因可能是马来酸酐的极性基团会给聚合物引入深陷阱，深陷阱的增加使得一些迁移的电荷在运动过程中被束缚，提高了注入势垒。
添加电压稳定剂是一种传统的电力电缆绝缘材料的改性方法，可以显著改善聚合物绝缘材料对电树枝的抑制和耐受能力[7]，而且电压稳定剂改性法具有廉价、易操作等优点，因此被广泛应用于XLPE绝缘电缆材料中[8]。尹毅等[9]对电压稳定剂如何抑制聚乙烯（PE）电树枝引发做了一系列的探究。结果表明，电压稳定剂可以通过改善PE的结晶状态来抑制电树枝的引发，并提出能有效改善PE聚集态结构的材料可以充当电压稳定剂。屠德民等[10]研究发现将弱电解质掺入聚合物中可提高其在高场强下的电导，若将此聚合物置于极不均匀电场中，由于聚合物的非线性电导特性使电场畸变程度下降，从而削弱了高电场对材料的破坏作用，抑制了电树枝的引发。李忠华等[11]通过试验证实了电压稳定剂能显著抑制XLPE电树枝的引发，提高XLPE的耐电能力。Y YAMANO等[12]研发了一系列稠环芳香烃化合物及其衍生物的电压稳定剂，分析了其对低密度聚乙烯（LDPE）直流电气强度与电树枝引发特性的影响。结果表明，这类电压稳定剂可改变PE分子的陷阱分布从而影响电荷的运动过程，当其连接受电子基团时，对其俘获电子的能力有很大的增强作用。
由于环保型电力电缆绝缘材料的概念是近几年提出并得到广泛关注的，环保型PP基绝缘材料的研究与应用时间尚短，针对电压稳定剂在环保型PP基绝缘材料中的应用尚无相关报道。若将电压稳定剂应用于PP基绝缘材料，则可以发挥电压稳定剂吸收高能电子的独特优势，有可能使得PP基绝缘材料的耐电性能得到大幅改善，这为环保可回收PP电缆绝缘材料的开发提供了进一步的改性思路。
理论化学计算表明，芳香酮类化合物大多具有较好的共轭特征与电子离域性，致使其电子亲和能普遍较高，且从其分子结构本身的化学特性来看，其不易和抗氧剂、交联剂等电缆绝缘必备的有机助剂相互抑制，可作为电缆绝缘的电压稳定剂。但是芳香酮类电压稳定剂分子量较小，在熔融共混的条件下掺杂在PP中，很难长期稳定地均匀分布在PP中，且容易发生迁移析出，有可能导致其作用效果逐渐退化。若将芳香酮类稳定剂分子接枝到PP大分子上，有可能可以克服其分散不均匀以及迁移挥发的问题[13]，从而保障稳定剂的长期作用效果。目前已有研究证实，使用少量过氧化物作为有机化合物接枝反应的引发剂，可在不影响材料热塑性的同时对材料进行接枝改性[14]。结合前期研究得到的一种可接枝电压稳定剂4-丙烯氧基-2-羟基二苯甲酮（AOHBP）[15]，本研究使用过氧化二异丙苯（DCP）作为接枝反应的引发剂，主要研究电压稳定剂AOHBP通过接枝反应连接到PP的大分子后对材料性能的影响。为了抑制DCP加入后对PP基绝缘材料电气性能的影响，本研究还添加了防降解添加剂苯乙烯衍生物（St），并探究其对材料电学性能的影响。
1 试验
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1.1 主要原材料
基料：聚丙烯，K8003型，中国石化有限公司；防降解添加剂：苯乙烯衍生物（St），Alfa Aesar公司；引发剂：过氧化二异丙苯（DCP），中国石化集团经营管理有限公司上海高桥分公司；电压稳定剂：4-丙烯氧基-2-羟基二苯甲酮（AOHBP），阿拉丁生化科技股份有限公司，分子式如图1所示。
1.2 试样制备
采用转矩流变仪进行混料，温度设置为200℃，转速为60 r/min。在混料过程中，为抑制PP在试验中发生降解，添加St作为辅助材料。将材料PP、St、AOHBP、DCP按顺序依次加入转矩流变仪进行混料，每种材料加入后混炼2 min，最终制得试样。不同试样的命名和配方如表1所示。
1.3 测试与表征
1.3.1 红外光谱
通过测试AOHBP接枝PP和AOHBP与PP共混两种不同改性方式得到的材料分别在70℃下真空脱气28 d后的红外吸收光谱变化，分析AOHBP分子是否接枝在PP上。测试仪器为FT/IR6100型红外光谱仪，测试波数范围为500～2 500 cm-1，分辨率为2 cm-1，试样厚度为200 μm。
1.3.2 熔融指数（MI）
熔融指数可以用于表征聚合物材料的分子量，也可以用于分析PP材料在高温加工过程中的降解程度。文献[19]指出，PP主链的降解反应增强会引起材料熔体流动速率的增大。为验证PP在接枝试验过程中是否降解，本研究测定了试样PP、PP+0.2DCP、PP+1St+0.2DCP和PP+1St+0.6AOHBP+0.2DCP的熔融指数（MI）。具体步骤为：先在转矩流变仪混料，然后在平板硫化仪上制备厚度为1 mm的正方形试样，再将试样剪成粒状粉末。打开XRZ-300型溶体流动速率仪，设置温度为230℃，待机器升温至恒温后，将准备好的试样粉末装入料筒，施加2.16 kg的负荷，测量材料熔体在10 min内在口模中流出的质量。每种试样重复测试3次，结果取平均值。
1.3.3 拉伸性能测试
利用拉伸试验可以进一步验证PP在试验过程中的降解程度及St对材料降解的抑制效果，试样种类与熔融指数试验相同。根据GB/T 2951.11—2008采用WDW-10C型试验机进行测试，试样总长度为75 mm，试验标距为（20.0±0.5）mm，有效测试部分宽度为（4.0±0.2）mm，厚度约为1 mm。拉伸速率为50 mm/min，测试温度为室温，每种材料重复测试5次，结果取平均值。
1.3.4 差示扫描量热法（DSC）
采用DSC822e型差示扫描量热仪测试AOHBP在接枝PP时对其结晶性能的影响。具体步骤为：称取试样5～10 mg置入标准坩埚中，放进仪器内的指定区域，通过吹入高纯氮气进行保护，吹入氮气的速率为150 mL/min，升温和降温速率均为10℃/min。为了消除材料热历史的影响，先设置升温温度范围为25～190℃，达到190℃后保持恒温5 min，再降温至60℃保持5 min，在此期间测试试样的结晶过程热流变化。然后由60℃升温至190℃，在此期间测试试样熔融过程的热流变化。结晶度Xc计算公式如（1）所示。
Xc=ΔHmΔH100×100%
式（1）中：ΔHm为试样的熔融热焓，J/g；ΔH100为试样结晶度为100%时的熔融热焓，本文PP取ΔH100=209 J/g[18]。
1.3.5 电树枝试验
经前期试验验证，AOHBP添加量为0.6份时对PP电树枝起始电压的提升效果最优，因此本研究选用添加量为0.6份的AOHBP来进行接枝PP的电树枝试验，同时试验过程中还选取了多个变量作为对照组，即接枝时是否添加St、共混材料是否添加St来探究St对材料的影响。电树枝试验采用针-板电极试样，针尖曲率半径约为5 μm，针尖距离接地电极3 mm，采用埋针法制备试样。由于所采用的K8003型PP透明度很低，本研究采用基于HFCT电流传感器检测电树枝引发时的局部放电电压来判定电树枝的引发电压。采用0.5 kV/s的速率升高电压，当出现大于5 pC的局部放电时即视为电树枝引发。用电树枝起始电压测试系统对10个试样进行电树枝引发测试，测得电树枝引发后的局部放电起始电压和熄灭电压，并采用双参数Weibull分布进行统计。
1.3.6 直流电气强度测试
经前期试验验证，AOHBP添加量为0.4份时对PP直流电气强度的提升效果最优，因此本研究选用添加量为0.4份的AOHBP接枝PP来进行接枝PP的直流电气强度测试。与电树枝试验相同，直流电气强度测试也选取了多个变量作为对照组。
直流电气强度测试采用圆柱电极，高压电极与接地电极直径分别为35 mm和50 mm且均带有 5 mm圆角，以防止在测试中发生局部放电影响试验结果，试样与高压电极接触面积的直径为25 mm。高压电极为环氧树脂包封电极，作用有两点：①在测试过程中减少闪络；②增大测试面积，充分暴露材料的内部缺陷以提高试验结果的准确度。试验时将片状试样置于上、下电极之间并浸没在硅油中，匀速加压直至试样击穿后读取击穿电压U，结合试样厚度d，根据公式E=U/d计算出对应的直流电气强度，每种材料至少测试15个试样，测得电气强度采用双参数Weibull分布进行统计。
2 结果与讨论
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2.1 红外光谱分析
文献[19]指出，AOHBP含有不饱和可接枝基团，能参与DCP引发的自由基反应，但在使用DCP作为接枝反应的引发剂时，PP上叔碳原子的氢原子很容易被引发剂夺走产生游离基，进而使PP降解，从而改变PP基绝缘材料的电气性能，因此其可接枝性需要进一步进行试验验证。本研究通过红外光谱验证电压稳定剂AOHBP的可接枝性。
PP+1St+0.6AOHBP和PP+1St+0.6AOHBP+0.2 DCP两种试样经过28 d真空脱气处理后的红外吸收光谱如图2所示。
从图2可知，在红外光谱中可以看到PP的典型特征吸收峰，其中PP+1St+0.6AOHBP试样在1 580 cm-1处由AOHBP分子苯环引起的吸收峰明显减弱，1 627 cm-1处由AOHBP分子芳香酮双键C=O双键伸缩震动产生的吸收峰大幅减小。从这两处特征峰的变化可以看出，未添加接枝引发剂DCP的试样在脱气后AOHBP已经迁移挥发，而含有接枝引发剂的材料中AOHBP还大量存在于混合物中，说明AOHBP成功接枝在PP的大分子上。
2.2 熔融指数
各PP试样熔融指数的测试结果如表2所示。由表2可知，与纯PP相比，PP+0.2DCP试样的流动速率很快，熔体不成型，其熔融指数很大，而PP+1St+0.2DCP试样的熔融指数显著下降，可见St的加入抑制了PP接枝试验过程中的降解。而加入0.6份AOHBP后，试样的熔融指数又进一步下降，可见AOHBP加入后可以和St共同作用，从而减缓材料的降解。
2.3 拉伸性能
各PP试样的应力-应变曲线见图3，具体数值见表3。
从图3和表3可以看出，与纯PP相比，PP+0.2DCP的断裂伸长率、拉伸断裂应力和拉伸屈服应力大幅下降，这是由于加入的引发剂DCP受热分解为活性很强的自由基，夺取了PP分子链中叔碳原子的氢原子，分子链断裂，使材料结构很不稳定；而在加入St后，由于St具有很强的自由基[18]，可以在PP降解之前优先接枝在自由基上，稳定大分子自由基，因此材料的断裂伸长率及拉伸屈服应力相较于只添加DCP的材料提高很多，但是还存在少许降解，因此力学性能稍差于纯PP；在接枝AOHBP之后，试样的拉伸强度相较于未接枝AOHBP的材料提高很多，并高于纯PP的拉伸强度，一方面可能是AOHBP进一步促进了St抑制材料降解的作用，从而避免大分子链的大量降解，另一方面可能是AOHBP上的两个苯环会使位阻增大，刚性基团引入后也会使PP的刚性增大，结晶度降低幅度较小，拉伸强度有所升高。综上所述，再次验证了St的加入可以很好地抑制PP在试验过程中的降解，从而提高接枝产物的力学性能。
2.4 差示扫描量热法（DSC）测试结果
各PP试样结晶和熔融过程的DSC曲线如图4所示，结晶参数见表4。首先分析PP、PP+0.2DCP、PP+1St+0.2DCP的结晶性能，由表4可知，加入引发剂DCP之后，PP大分子降解，结晶度下降；而加入St之后，结晶度有所上升，但仍低于纯PP，说明在DCP的作用下St的加入使材料的结晶行为被抑制，这是因为St的苯环结构抑制了大分子的规则排列，从而降低了材料的结晶度，片晶厚度减小；其熔融峰温度和结晶峰温度与纯PP比较有轻微下降，说明St的引入使材料的结晶难度变大，结晶容易融化。对比PP、PP+0.2DCP、PP+1St+0.2DCP的半熔融峰宽度发现，PP+0.2DCP的峰要宽于纯PP和PP+1St+0.2DCP，而纯PP的峰要比PP+1St+0.2DCP略宽一些，原因可能是DCP的引入使PP降解，因为降解前分子链的长短相对统一，而部分降解后材料内分子降解程度不同，分子链长短不一，使得结晶峰变宽，即使加入St后也没有完全抑制降解，因此再次验证了St的加入可以抑制材料的降解。
对比PP+1St+0.2DCP与PP+1St+0.6AOHBP+ 0.2DCP的测试结果发现，AOHBP的加入使试样的结晶度由40.0%降低到了39.6%，在DSC曲线中表示为熔融峰和结晶峰的面积减小，说明AOHBP的加入进一步抑制了材料的结晶过程，其主要原因可能是AOHBP在DCP引发的反应进程中会通过其乙烯基上的加成反应接枝到PP大分子上，AOHBP分子接枝后进一步破坏了PP分子链的规整性，因此结晶过程中大分子的规则堆砌被进一步抑制，AOHBP对PP结晶性能的影响规律可以作为AOHBP可接枝性的又一佐证。而其熔融峰温度有所上升，结晶峰温度变化不大，说明片晶厚度变厚，结晶相对来说不易融化。再观察接枝AOHBP后试样的熔融峰宽度发现，与未接枝AOHBP之前相比有所变窄，说明AOHBP促进了St抑制降解的作用。综上所述，再次验证了AOHBP的可接枝性，St具有较优的抑制降解效果，且AOHBP的接入会促进St抑制降解的作用。
2.5 电树枝起始电压
电树枝引发过程中的局部放电起始电压和熄灭电压如图5和图6所示，具体数据如表5所示。
从表5可以看出，与PP+0.6AOHBP相比，PP+1St+0.6AOHBP的电树枝局部放电起始电压和熄灭电压均降低，起始电压从10.1 kV下降至7.5 kV，熄灭电压从4.4 kV下降至3.1 kV，甚至低于纯PP的电树枝起始电压和熄灭电压。PP+0.6AOHBP+0.2DCP试样的起始电压和熄灭电压下降更明显，与纯PP相比，分别下降了3.9%、9.1%，这是由于在使用DCP作为接枝反应的引发剂时，PP上叔碳原子的氢原子很容易被引发剂夺走产生游离基，进而使PP降解，从而降低PP的电气性能。PP+1St+0.2DCP试样的起始电压和熄灭电压相比于纯PP分别下降了1.3%、6.1%；但PP+1St+0.6AOHBP+0.2DCP试样的电树枝起始电压和熄灭电压都提高了很多，比PP+0.6AOHBP+0.2DCP试样提高了30.1%、30.0%，比纯PP提高了25.0%、18.2%。这是由于St在引发剂DCP前加入，先稳定了材料的大分子自由基，抑制了材料的降解，并且改性后PP中的AOHBP作为芳香酮分子，相较于饱和的PP具有更高的电子亲合能以及更低的电离势，电子在电场作用下注入并加速的过程中将有较大的概率与AOHBP发生碰撞，俘获高能电子，一定程度上抑制了局部放电的发生，进而提高了PP的电树枝起始电压[19]。
从表5还可以看出，电压稳定剂接枝改性材料相比仅物理共混电压稳定剂的PP材料（PP+0.6AOHBP）耐电树枝性能均有一定程度下降；若不使用St，则接枝电压稳定剂无法提高材料的耐电树枝性能；若接枝引发剂、St和电压稳定剂三者不共同作用，也无法改善材料的耐电树枝性能。这些试验现象说明，PP材料加工过程（接枝反应进程）中的大分子降解对于材料耐电树枝性能有显著影响，电压稳定剂抑制电树枝的效果容易被大分子降解所破坏，St本身未能体现出对耐电树枝性能的改善效果，但其作为抑制降解的添加剂，保障了电压稳定剂的自由基接枝反应，使得PP基体材料的大分子仅发生少量降解，从而使得电压稳定剂接枝后的作用效果仍能大幅度保持。
2.6 直流电气强度
各试样的直流电气强度测试结果如图7所示，图中尺度表示击穿概率为63.2%时对应的电气强度。从图7可以看出，与PP+0.4AOHBP相比，PP+1St+0.4AOHBP的直流电气强度从354.5 kV/mm降低至320.5 kV/mm，但仍高于纯PP的直流电气强度。当PP仅在DCP作用下接枝0.4份AOHBP时，试样的直流电气强度下降更加明显，相比于纯PP还降低了5.5%；但材料如果在接枝反应前先加入了St，由于St在引发剂DCP前加入，先稳定了材料的大分子自由基，抑制了材料的降解，材料的直流电气强度提高了很多，比未加St前提高了21.9%，比纯PP提高了15.2%。由此可见，电压稳定剂在St和DCP作用下完成接枝PP大分子的反应后，可以提高PP的直流电气强度。总体来看，无论是物理共混还是接枝反应，电压稳定剂均能提高PP的直流电气强度，这是因为AOHBP相较于饱和的PP具有更高的电子亲合能和较窄的能隙，较高的电子亲和能使AOHBP有更大概率俘获高能电子，较窄的能隙可以将吸收的能量以光能或内能两种危害相对较小的形式释放出去，因此AOHBP改性后，材料中的高能电子对PP大分子链轰击的概率降低，破坏作用大幅削弱，电气强度显著提升。但电压稳定剂接枝改性材料相比仅物理共混电压稳定剂的PP材料直流电气强度有一定程度下降；若不使用St，则接枝电压稳定剂无法提高材料的直流电气强度；即使不共同使用接枝引发剂、St和电压稳定剂，也可以一定程度地提高纯PP材料的直流电气强度，这与电压稳定剂抑制电树枝引发试验的规律不同，其原因可能是相比于电树枝引发，材料的直流电气强度受St影响的敏感程度下降。这些试验现象还说明，PP材料在接枝反应进程中的大分子降解对于材料直流击穿性能有十分显著的影响；电压稳定剂改善材料直流击穿性能的效果容易被大分子降解所破坏；St本身没有体现出对材料直流击穿性能的改善效果，但其作为抑制降解的添加剂，保障了电压稳定剂自由基接枝反应后，PP基体材料的大分子仅发生少量降解，从而使得电压稳定剂接枝后的作用效果仍能保持，虽未达到相同组分PP共混电压稳定剂的直流电气强度，但材料接枝后良好的耐迁出稳定性要优于共混PP/电压稳定剂共混绝缘材料，因此接枝电压稳定剂的PP基绝缘材料亦有很高的研究价值。
3 结论
收起
（1）AOHBP作为可接枝型电压稳定剂，在DCP引发的自由基接枝反应过程中，AOHBP可以通过自由基反应接枝到PP上，且接枝后具有良好的耐迁出稳定性。
（2）加入苯乙烯衍生物St可抑制PP接枝反应过程中的降解，降低聚合物的熔融指数，提高其断裂伸长率，AOHBP的加入可以增强St抑制PP大分子降解的作用。
（3）常温下AOHBP在防降解材料St的辅助下接枝改性PP可以提高其电树枝起始电压和直流电气强度，相比于未接枝的AOHBP与PP共混物，电压稳定剂作用效果有所降低。
基金
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  • 国家自然科学基金资助项目(U20A200815)
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doi: 10.16790/j.cnki.1009-9239.im.2022.05.005
  • 接收时间：2021-07-13
  • 首发时间：2025-12-22
  • 出版时间：2022-05-20
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  • 收稿日期：2021-07-13
  • 修回日期：2021-09-12
基金
国家自然科学基金资助项目(U20A200815)
作者信息
    1哈尔滨理工大学 工程电介质及其应用技术教育部重点实验室,黑龙江 哈尔滨 150080
    2国网内蒙古东部电力有限公司赤峰供电公司,内蒙古 赤峰 024000
    3浙江晨光电缆股份有限公司,浙江 平湖 314204

通讯作者:

李春阳（1991-），男（汉族），黑龙江哈尔滨人，讲师，研究方向为高压电力电缆及其附件用聚合物绝缘材料。
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
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