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Article(id=1304921757471756716, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304921635748864029, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2026.07.010, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1753200000000, receivedDateStr=2025-07-23, revisedDate=1757779200000, revisedDateStr=2025-09-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1789047191254, onlineDateStr=2026-09-10, pubDate=1784476800000, pubDateStr=2026-07-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1789047191254, onlineIssueDateStr=2026-09-10, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1789047191254, creator=13701087609, updateTime=1789047191254, updator=13701087609, issue=Issue{id=1304921635748864029, tenantId=1146029695717560320, journalId=1149653034449285133, year='2026', volume='59', issue='7', pageStart='1', pageEnd='160', issueExtLink='null', onlineDate='null', pubDate='1784476800000', pubDateStr='2026-07-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1789047162234, creator='13701087609', updateTime=1789117876219, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1305218231761920521, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304921635748864029, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1305218231761920522, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304921635748864029, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=86, endPage=93, ext={EN=ArticleExt(id=1304921757949907373, articleId=1304921757471756716, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Performance evaluation and combined electro-thermal ageing characteristics of BOPP films based on domestically washed polypropylene resins, columnId=1190369198472794288, journalTitle=Insulating Materials, columnName=Insulation Technology, runingTitle=null, highlight=null, articleAbstract=

To address the key problems in ultra-high voltage flexible DC transmission system that the core biaxially oriented polypropylene (BOPP) films for dry-type DC capacitors rely on imports, and the high ash content of domestic polypropylene resins leads to insufficient insulation and ageing resistance of the films, we selected imported electrical-grade, domestic continuously washed low-ash, and domestic unwashed high-ash polypropylene resins to prepare BOPP films. The microscopic morphology, crystal structure and electrical properties of the films were characterized systematically, and the combined electro-thermal ageing tests under AC-DC superimposed conditions were conducted. The results show that BOPP films prepared from low-ash domestic washed polypropylene resin have higher electric strength and more stable high-temperature dielectric performance. Moreover, the crystal structure of the films has no significant changes after ageing, and their electrical properties are close to those of the imported BOPP films.

, authors=Yaotian Su, Bo Yang, Chong Zhang, Shaowei Guo, Juyang Liu, Bo Wang, Zhaoliang Xing*, authorsList=Yaotian Su, Bo Yang, Chong Zhang, Shaowei Guo, Juyang Liu, Bo Wang, Zhaoliang Xing, authorCompany=null, correspAuthors=Zhaoliang Xing, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1304921762236486088, articleId=1304921757471756716, tenantId=1146029695717560320, journalId=1149653034449285133, language=CN, title=基于国产洗涤聚丙烯树脂的BOPP薄膜性能测试及电-热联合老化特性研究, columnId=1190369198724452531, journalTitle=绝缘材料, columnName=绝缘技术, runingTitle=null, highlight=null, articleAbstract=

为解决特高压柔性直流输电系统中干式直流电容器用双向拉伸聚丙烯（BOPP）薄膜依赖进口、国产聚丙烯树脂灰分含量偏高导致薄膜绝缘及耐老化性能不足的关键问题，本文选取进口电工级、国产连续洗涤低灰分、国产未洗涤高灰分聚丙烯树脂制备BOPP薄膜，系统表征了薄膜微观形貌、结晶结构与电学特性，并开展了交-直流叠加电-热联合老化试验。结果表明：低灰分国产洗涤聚丙烯树脂制备的BOPP薄膜具有更高的电气强度和更稳定的高温介电性能，且老化后薄膜晶区结构无显著变化，电学性能接近进口BOPP薄膜水平。

, authors=苏尧天, 杨博, 张翀, 郭少玮, 刘炬阳, 王博, 邢照亮*, authorsList=苏尧天, 杨博, 张翀, 郭少玮, 刘炬阳, 王博, 邢照亮, authorCompany=null, correspAuthors=邢照亮, authorNote=

苏尧天（1990-），男（汉族），河北保定人，工程师，博士，主要从事绝缘电介质材料的研究工作

, correspAuthorsNote=
邢照亮（1988-），男（汉族），山东临沂人，高级工程师，主要从事绝缘电介质材料的研究工作。
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苏尧天（1990-），男（汉族），河北保定人，工程师，博士，主要从事绝缘电介质材料的研究工作

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苏尧天（1990-），男（汉族），河北保定人，工程师，博士，主要从事绝缘电介质材料的研究工作

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Chemical Engineering Journal,2024,492:152237., articleTitle=Thin, large-scale processed, high-temperature resistant capacitor films based on polypropylene/cycloolefin copolymer blend, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1304921762622362057, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, xref=null, ext=[AuthorCompanyExt(id=1304921762630750666, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, companyId=1304921762622362057, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=State Key Laboratory of Advanced Power Transmission Technology, China Electric Power Research Institute Co., Ltd., Beijing 102209, China), AuthorCompanyExt(id=1304921762639139275, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, companyId=1304921762622362057, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中国电力科学研究院有限公司 先进输电技术全国重点实验室，北京　102209)])], figs=[ArticleFig(id=1304921768838320635, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.1, caption=Schematic diagram of washing and recycling process, figureFileSmall=TeoW8bRke9Be8aX9H7ohJg==, figureFileBig=bs7eQsElfLI0FaKT2cAfIg==, tableContent=null), ArticleFig(id=1304921769215807996, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图1, caption=洗涤及回收流程示意图, figureFileSmall=TeoW8bRke9Be8aX9H7ohJg==, figureFileBig=bs7eQsElfLI0FaKT2cAfIg==, tableContent=null), ArticleFig(id=1304921770037891581, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.2, caption=Schematic diagram of asynchronous biaxial stretching process, figureFileSmall=SAEIg46KkmLnamYwvc74nA==, figureFileBig=D49REdwBeSQzMPnYL75tyA==, tableContent=null), ArticleFig(id=1304921770134360576, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图2, caption=异步双向拉伸工艺示意图, figureFileSmall=SAEIg46KkmLnamYwvc74nA==, figureFileBig=D49REdwBeSQzMPnYL75tyA==, tableContent=null), ArticleFig(id=1304921770448933377, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.3, caption=Schematic diagram of electro-thermal combined ageing platform, figureFileSmall=5DG3mFtXavGqZa5j3iVK7Q==, figureFileBig=G2L6Vbsr/vNAKLwF16afgg==, tableContent=null), ArticleFig(id=1304921770511847938, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图3, caption=电-热联合老化平台示意图, figureFileSmall=5DG3mFtXavGqZa5j3iVK7Q==, figureFileBig=G2L6Vbsr/vNAKLwF16afgg==, tableContent=null), ArticleFig(id=1304921770574762499, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.4, caption=Surface morphologies of different BOPP films before and after ageing, figureFileSmall=son3/Md/Zle3bJtW3SuVXQ==, figureFileBig=IapxK7/5g34Y6yccpHOrRQ==, tableContent=null), ArticleFig(id=1304921770885140996, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图4, caption=老化前后不同BOPP薄膜表面形貌, figureFileSmall=son3/Md/Zle3bJtW3SuVXQ==, figureFileBig=IapxK7/5g34Y6yccpHOrRQ==, tableContent=null), ArticleFig(id=1304921771296182789, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.5, caption=Statistics on the number and size of "crater" on the surface of different BOPP films, figureFileSmall=YbraxKcfq4VYpF5rMgPSiA==, figureFileBig=iJi5GR/gkGdcRrYoyYU6Sg==, tableContent=null), ArticleFig(id=1304921771401040390, tenantId=1146029695717560320, journalId=1149653034449285133, 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after ageing, figureFileSmall=04tfCBq8v3AA4kgQ4/kVgw==, figureFileBig=v9/H0Dr46HPEyXz7Ag8RDw==, tableContent=null), ArticleFig(id=1304921772223123978, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图7, caption=老化前后不同BOPP薄膜DSC曲线, figureFileSmall=04tfCBq8v3AA4kgQ4/kVgw==, figureFileBig=v9/H0Dr46HPEyXz7Ag8RDw==, tableContent=null), ArticleFig(id=1304921772554473995, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.8, caption=Weight-average molecular weight of different BOPP films before and after ageing, figureFileSmall=rNWPCCghXOv0+qmwTpNsZA==, figureFileBig=Sh7hdxS96lNYV7kwWDUBTA==, tableContent=null), ArticleFig(id=1304921772625777164, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图8, caption=老化前后不同BOPP薄膜的重均分子量变化, figureFileSmall=rNWPCCghXOv0+qmwTpNsZA==, figureFileBig=Sh7hdxS96lNYV7kwWDUBTA==, tableContent=null), ArticleFig(id=1304921772688691725, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.9, caption=Capacity attenuation of different film capacitors before and after ageing, figureFileSmall=K7zCD2VwUiJAO5SYfrREOg==, figureFileBig=+BO/qDgl77P/pc+451SisA==, tableContent=null), ArticleFig(id=1304921773015847438, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图9, caption=老化前后不同薄膜电容器容量衰减, figureFileSmall=K7zCD2VwUiJAO5SYfrREOg==, figureFileBig=+BO/qDgl77P/pc+451SisA==, tableContent=null), ArticleFig(id=1304921773074567695, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.10, caption=Broadband dielectric spectra of different BOPP films at 85℃ before and after ageing, figureFileSmall=F0eZ+pfESNJHfqWDLuU/Zw==, figureFileBig=neELaaTOJecXcJXx0ZdNLg==, tableContent=null), ArticleFig(id=1304921773141676560, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图10, caption=老化前后不同BOPP薄膜在85℃下的宽频介电谱, figureFileSmall=F0eZ+pfESNJHfqWDLuU/Zw==, figureFileBig=neELaaTOJecXcJXx0ZdNLg==, tableContent=null), ArticleFig(id=1304921773447860753, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Fig.11, caption=DC electric strength of different BOPP films at 85℃ before and after ageing, figureFileSmall=iUE/2px23/YLRResvek+8Q==, figureFileBig=uTV8yibJJebqe+jdBSygNg==, tableContent=null), ArticleFig(id=1304921773531746834, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=图11, caption=不同BOPP薄膜老化前后在85℃下的直流电气强度, figureFileSmall=iUE/2px23/YLRResvek+8Q==, figureFileBig=uTV8yibJJebqe+jdBSygNg==, tableContent=null), ArticleFig(id=1304921773804376595, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Table 1, caption=

Key parameters of three polypropylene resins

, figureFileSmall=null, figureFileBig=null, tableContent=
性能指标样品
PP-1PP-2PP-3
熔融指数/(g/10min)3.43.23.1
等规度/%99.298.897.5
灰分/(×10-6)161632
重均分子量(Mw)350 000339 000336 000
分子量分布(PDI)6.44.24.6
), ArticleFig(id=1304921773858902548, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=表1, caption=

3种聚丙烯树脂的主要参数

, figureFileSmall=null, figureFileBig=null, tableContent=
性能指标样品
PP-1PP-2PP-3
熔融指数/(g/10min)3.43.23.1
等规度/%99.298.897.5
灰分/(×10-6)161632
重均分子量(Mw)350 000339 000336 000
分子量分布(PDI)6.44.24.6
), ArticleFig(id=1304921773946982933, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Table 2, caption=

Properties of different BOPP films

, figureFileSmall=null, figureFileBig=null, tableContent=
性能指标要求值样品
BP-1BP-2BP-3
电子测厚/μm5.8±0.125.85.85.8
粗糙度(Ra)/μm0.08±0.020.0850.0720.096
热收缩率/%(MD, 120℃)≤3.52.43.13.3
纵向拉伸强度/MPa≥150166156151
横向拉伸强度/MPa≥280298292305
), ArticleFig(id=1304921774060229143, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=表2, caption=

不同双向拉伸聚丙烯薄膜的性能

, figureFileSmall=null, figureFileBig=null, tableContent=
性能指标要求值样品
BP-1BP-2BP-3
电子测厚/μm5.8±0.125.85.85.8
粗糙度(Ra)/μm0.08±0.020.0850.0720.096
热收缩率/%(MD, 120℃)≤3.52.43.13.3
纵向拉伸强度/MPa≥150166156151
横向拉伸强度/MPa≥280298292305
), ArticleFig(id=1304921774223807000, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Table 3, caption=

Crystallization parameters of different BOPP films before and after electro-thermal ageing

, figureFileSmall=null, figureFileBig=null, tableContent=
样品结晶度/%片晶尺寸/nm
BP-1老化前52.513.49
BP-1老化后54.613.98
BP-2老化前51.213.16
BP-2老化后52.314.10
BP-3老化前50.413.12
BP-3老化后52.613.48
), ArticleFig(id=1304921774316081689, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=表3, caption=

电-热老化前后不同BOPP薄膜结晶参数对比

, figureFileSmall=null, figureFileBig=null, tableContent=
样品结晶度/%片晶尺寸/nm
BP-1老化前52.513.49
BP-1老化后54.613.98
BP-2老化前51.213.16
BP-2老化后52.314.10
BP-3老化前50.413.12
BP-3老化后52.613.48
), ArticleFig(id=1304921774387384858, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=EN, label=Table 4, caption=

Dielectric response parameters of different BOPP films before and after ageing

, figureFileSmall=null, figureFileBig=null, tableContent=
指标BP-1BP-2BP-3
老化前老化后老化前老化后老化前老化后
介电常数2.212.222.232.242.302.34
介质损耗因数0.003 00.003 40.002 80.003 20.003 20.005 1
), ArticleFig(id=1304921774458688027, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304921757471756716, language=CN, label=表4, caption=

老化前后不同BOPP薄膜介电响应参数

, figureFileSmall=null, figureFileBig=null, tableContent=
指标BP-1BP-2BP-3
老化前老化后老化前老化后老化前老化后
介电常数2.212.222.232.242.302.34
介质损耗因数0.003 00.003 40.002 80.003 20.003 20.005 1
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基于国产洗涤聚丙烯树脂的BOPP薄膜性能测试及电-热联合老化特性研究
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苏尧天 , 杨博 , 张翀 , 郭少玮 , 刘炬阳 , 王博 , 邢照亮 *
绝缘材料 | 绝缘技术 2026,59(7): 86-93
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绝缘材料 |绝缘技术 2026 , 59 (7) : 86 -93
基于国产洗涤聚丙烯树脂的BOPP薄膜性能测试及电-热联合老化特性研究
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苏尧天（1990-），男（汉族），河北保定人，工程师，博士，主要从事绝缘电介质材料的研究工作

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苏尧天, 杨博, 张翀, 郭少玮, 刘炬阳, 王博, 邢照亮*
作者信息
  • 中国电力科学研究院有限公司 先进输电技术全国重点实验室，北京　102209
通讯作者:
邢照亮（1988-），男（汉族），山东临沂人，高级工程师，主要从事绝缘电介质材料的研究工作。
作者简介:

苏尧天（1990-），男（汉族），河北保定人，工程师，博士，主要从事绝缘电介质材料的研究工作

Performance evaluation and combined electro-thermal ageing characteristics of BOPP films based on domestically washed polypropylene resins
Yaotian Su, Bo Yang, Chong Zhang, Shaowei Guo, Juyang Liu, Bo Wang, Zhaoliang Xing*
Affiliations
  • State Key Laboratory of Advanced Power Transmission Technology, China Electric Power Research Institute Co., Ltd., Beijing 102209, China
出版时间: 2026-07-20 doi: 10.16790/j.cnki.1009-9239.im.2026.07.010
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摘要
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为解决特高压柔性直流输电系统中干式直流电容器用双向拉伸聚丙烯（BOPP）薄膜依赖进口、国产聚丙烯树脂灰分含量偏高导致薄膜绝缘及耐老化性能不足的关键问题，本文选取进口电工级、国产连续洗涤低灰分、国产未洗涤高灰分聚丙烯树脂制备BOPP薄膜，系统表征了薄膜微观形貌、结晶结构与电学特性，并开展了交-直流叠加电-热联合老化试验。结果表明：低灰分国产洗涤聚丙烯树脂制备的BOPP薄膜具有更高的电气强度和更稳定的高温介电性能，且老化后薄膜晶区结构无显著变化，电学性能接近进口BOPP薄膜水平。

直流电容器  /  聚丙烯  /  连续洗涤  /  灰分  /  老化实验

To address the key problems in ultra-high voltage flexible DC transmission system that the core biaxially oriented polypropylene (BOPP) films for dry-type DC capacitors rely on imports, and the high ash content of domestic polypropylene resins leads to insufficient insulation and ageing resistance of the films, we selected imported electrical-grade, domestic continuously washed low-ash, and domestic unwashed high-ash polypropylene resins to prepare BOPP films. The microscopic morphology, crystal structure and electrical properties of the films were characterized systematically, and the combined electro-thermal ageing tests under AC-DC superimposed conditions were conducted. The results show that BOPP films prepared from low-ash domestic washed polypropylene resin have higher electric strength and more stable high-temperature dielectric performance. Moreover, the crystal structure of the films has no significant changes after ageing, and their electrical properties are close to those of the imported BOPP films.

DC capacitor  /  polypropylene  /  continuous washing  /  ash content  /  ageing experiment
苏尧天, 杨博, 张翀, 郭少玮, 刘炬阳, 王博, 邢照亮. 基于国产洗涤聚丙烯树脂的BOPP薄膜性能测试及电-热联合老化特性研究. 绝缘材料, 2026 , 59 (7) : 86 -93 . DOI: 10.16790/j.cnki.1009-9239.im.2026.07.010
Yaotian Su, Bo Yang, Chong Zhang, Shaowei Guo, Juyang Liu, Bo Wang, Zhaoliang Xing. Performance evaluation and combined electro-thermal ageing characteristics of BOPP films based on domestically washed polypropylene resins[J]. Insulating Materials, 2026 , 59 (7) : 86 -93 . DOI: 10.16790/j.cnki.1009-9239.im.2026.07.010
正文
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0　引言
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特高压柔性直流输电技术作为解决我国能源分布不均问题、实现跨区域大规模电力输送的核心手段，在保障能源安全、推动新能源并网等方面发挥着不可替代的作用[1-3]。而在特高压柔直输电系统中，电容器作为能量缓冲与电压支撑的关键设备，其性能稳定性直接关乎整个系统的安全高效运行。双向拉伸聚丙烯（BOPP）薄膜因具有优异的介电性能、机械强度和耐老化性，成为干式直流支撑电容器的核心介质材料，其品质直接决定了电容器的使用寿命、绝缘可靠性及运行效率[4-6]。然而，目前我国特高压柔直工程中所使用的高性能BOPP薄膜过度依赖进口，国产BOPP薄膜在介质损耗、耐电热老化性能等关键指标上与国际先进水平存在差距，尤其在灰分控制、分子链规整性等方面存在技术瓶颈，导致其难以满足特高压场景下的严苛工作要求，成为制约我国电力装备自主化的“卡脖子”难题[7-10]。突破国产BOPP薄膜的性能限制，实现其在特高压领域的规模化应用，对于提升我国电力工业核心竞争力、保障能源装备安全具有重要战略意义。
灰分是指产品经高温（850℃左右）灼烧后残留的杂质，作为衡量聚丙烯树脂及BOPP薄膜质量的关键指标，近年来受到学界与产业界的广泛关注。在聚丙烯树脂合成过程中，催化剂体系、聚合工艺以及原料纯度等因素共同作用于灰分的产生与积累。国内研究指出，传统催化剂制备的聚丙烯树脂灰分较高，在后续加工成膜时易造成熔体压力波动，不仅增加过滤网更换频率，还会影响薄膜微观结构的均匀性[11]。对于BOPP薄膜，灰分影响其介电性能、力学性能与耐老化性能等多个关键指标。在介电性能方面，高灰分薄膜在电场作用下易发生局部电场畸变，导致介质损耗增加，进而降低电容器的能量转换效率与使用寿命[12]。在力学性能上，灰分颗粒作为应力集中点，削弱分子链间的作用力，导致薄膜拉伸强度和韧性下降[13]。从耐老化性能来看，灰分可能加速氧化、热降解等老化进程，缩短薄膜实际服役时间[14]。尽管已有诸多研究对灰分控制与性能优化进行了探讨，但在国产聚丙烯树脂用于特高压柔直工程BOPP薄膜制备中，与灰分相关的关键技术难题仍待进一步攻克，亟需深入研究以缩小与国际先进水平的差距。
本文以连续洗涤纯化工艺制备的国产聚丙烯树脂为研究对象，对比分析国内外不同灰分含量树脂的常规理化性能，系统探究由其制备的BOPP薄膜在交-直流叠加电-热老化前后的性能变化规律，明晰灰分含量对薄膜微观结构与电学特性的作用机制。期望通过本研究验证低灰分国产聚丙烯树脂的制备与应用可行性，为特高压柔性直流输电用干式直流支撑电容器介质材料的国产化研发、性能提升及工程化应用提供实验支撑与参考依据。
1　实验
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1.1　主要原材料
进口电工级聚丙烯树脂（PP-1），牌号为HC312BF，北欧化工。国产连续洗涤纯化电工级聚丙烯树脂（PP-2），牌号为CA03BF，兰州石化。国产工业级聚丙烯树脂（PP-3），牌号为LB03F，兰州石化。3种树脂的理化性能如表1所示。
1.2　低灰分国产聚丙烯树脂制备
国产低灰分聚丙烯树脂PP-2通过原料精制和高活性催化剂等技术实现丙烯高效本体聚合，并经烷烃、醇类复配溶剂连续深度洗涤，实现了树脂灰分含量的显著下降。洗涤工艺如图1所示。洗涤溶剂采用正己烷与异丙醇复配体系，二者体积比为15∶4，洗涤温度控制在40～65℃，系统溶剂循环量为16～20 t/h。从表1可以看出，国产树脂PP-2灰分较PP-3下降了50%，此外由于洗涤也脱除了少量无规共聚物，使得PP-2等规度较PP-3提升了1.3%。
1.3　BOPP薄膜制备
采用异步双向拉伸工艺（如图2所示）将PP-1、PP-2、PP-3树脂制备成BOPP薄膜，分别命名为BP-1、BP-2、BP-3，其主要性能如表2所示。
1.4　主要仪器和设备
DSC-Q2000型差示扫描量热仪、DMA-Q800型动态热机械分析仪，美国TA公司；DM2700P型偏光显微镜，美国Leica公司；Xeuss2.0型广角X射线衍射仪（WAXD），法国Xenocs公司；PL-GPC220型高温凝胶渗透色谱仪，美国Agilent公司；HCDJC型直流击穿测试设备，北京华测试验仪器公司；Concept40型宽频介电谱仪，德国Novocontrol GmbH公司；6517B型灵敏电流计，美国Keithley公司；本实验所用交直流老化平台为自行搭建。
1.5　测试方法
1.5.1　差示扫描量热（DSC）分析
用分析天平称取7～8 mg薄膜样品，使用差示扫描量热仪以10℃/min速率升温至230℃得到升温曲线，进而得到熔融峰温度，按式（1）[15]计算结晶度（XC）。
XC=ΔHmΔHm,0×100%
式（1）中：ΔHm为样品的熔融焓，所取面积温度区间为120～190℃；ΔHm,0为聚丙烯α晶体100%结晶的熔融焓，取209 J/g。
1.5.2　偏光显微镜（POM）测试
取单层薄膜样品置于显微镜载物台的玻璃片上，在室温下直接采用透射模式对薄膜表面结构进行观察，并统计相同放大倍数下视野中“火山口”的数量。
1.5.3　广角X射线衍射（XRD）分析
采用X射线衍射仪对薄膜样品的晶型进行表征，测试的衍射角范围为10°～30°，根据布拉格公式计算晶体各参数，如式（2）[16]所示。
2d⋅sinθ=nλ
式（2）中：n为反射级数；θ为X射线入射线与衍射线的夹角；d为晶面间距；λ为入射X射线的波长。
1.5.4　高温凝胶渗透色谱（GPC）分析
将样品在160℃下、三氯苯中充分溶解后配置成浓度为1 mg/mL的聚合物溶液，采用高温凝胶渗透色谱仪对溶液进行表征。测试温度为150℃，进样体积为200 μL。通过校正曲线，将洗脱时间转化为分子量，得到分子量分布曲线。
1.5.5　电学性能测试
采用直流击穿设备测试材料在85℃下的电气强度，采用直径为25 mm的柱状铜电极进行测试，升压速率为200 V/s，测量50个点、结果取平均值，再除以样品厚度得到薄膜的电气强度。采用接触三电极法在85℃、10～105 Hz下对样品进行介电性能测试，样品采用50层薄膜叠层制成。
1.5.6　电-热老化实验
电-热老化平台示意图如图3所示，依据干式直流支撑电容器实际运行场强及GB/T 17702—2021要求，分别使用BP-1、BP-2、BP-3薄膜制成电容器样品（分别命名为FC-1、FC-2、FC-3），在80℃环境温度下，施加1.25倍直流额定电压（UNDC）与0.35倍交流额定电压（UNAC）的交-直流叠加电压，持续老化1 000 h，老化完成后拆解电容器，取出薄膜样品开展后续性能测试。
2　结果与讨论
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2.1　薄膜形貌
不同薄膜电-热老化前后的表面形貌如图4所示。从图4可以看出，电-热老化前后所有薄膜样品表面均呈现BOPP薄膜特有的圈状粗化环结构，这是双向拉伸过程中发生的β晶型向α晶型转变导致的现象。双向拉伸过程中的晶型转化导致薄膜的表面分子链堆叠形态和体积发生变化，进而形成大量细密的“火山口”形貌结构。
对“火山口”个数和尺寸进行统计，结果如图5所示。从图5可以看出，进口树脂制备的薄膜BP-1“火山口”个数更多，尺寸更小，直径集中分布于160～200 μm。对于国产树脂制备的薄膜BP-2“火山口”直径更大，分布于240～260 μm，而高灰分薄膜BP-3的“火山口”直径分布在300～320 μm。此外，通过对比电-热老化前后薄膜表面形貌，发现老化不会对膜面结构产生显著影响。通过以上分析可以推断，灰分是影响薄膜表面“火山口”数量和尺寸的重要因素。
2.2　结晶结构
聚丙烯的聚集态结构是由PP分子链在一定条件下堆叠形成的结晶区和无定形区并存的形态，其中晶区分子链长程有序紧密排列，无定形区则仅具有短程有序结构且分子链较松散。为研究聚丙烯薄膜的结晶特性，采用X射线衍射仪（XRD）和差示扫描量热仪（DSC）获取不同灰分含量国产和进口树脂制备的BOPP薄膜电-热老化前后的XRD谱图，如图6所示。
从图6可以看出，XRD图中的3个衍射峰分别对应于α晶型的（110）、（040）、（130）晶面，均未发现有β晶型的衍射峰，说明灰分含量和老化不会影响BOPP薄膜的晶型结构[16]。
薄膜的片晶尺寸（Δ）可通过对谱图中（040）衍射峰进行进一步分析，根据Debye-Scherre公式得到，如式（3）所示。
Δ=Kλβ(040)cosθ
式（3）中：K为Scherrer形状因子，取0.89；θ为Bragg角；β(040)为（040）衍射峰的半峰高宽度。
薄膜的结晶度可通过对衍射峰面积进行积分得到，如式（4）所示。
XC=S2-S1S1
式（4）中：S1为衍射图谱中整个衍射峰的面积；S2为非晶区的面积。
计算得到样品结晶度及片晶尺寸数据如表3所示。从表3可以看出，电-热老化前，BP-3的结晶度为50.4%、片晶尺寸为13.12 nm，不仅低于BP-2的51.2%和13.16 nm，也小于BP-1的52.5%和13.49 nm。经电-热老化处理后，所有BOPP薄膜的结晶度与片晶尺寸均呈增大趋势，其中BP-2薄膜变化尤为显著：其片晶尺寸提升幅度达7.1%，而BP-1和BP-3的片晶尺寸增幅分别为3.6%和2.7%。
采用DSC表征薄膜结晶度的变化，结果如图7所示。从图7可以看出，老化后所有BOPP薄膜的熔融温度均向高温方向移动，这归因于薄膜在电-热老化过程中片晶厚度的增加。不同灰分含量薄膜的DSC曲线特征差异主要体现在BP-1的熔融峰温度高于BP-2和BP-3。BP-2与BP-1熔融峰温度存在差异的主要原因在于，尽管BP-2灰分经洗涤后达到和BP-1含量相同水平，但是由于等规度和分子量分布差异使其结晶性仍未达到BP-1水平。
从图7还可以看出，BP-2熔融峰温度上升幅度比BP-3更大，这一现象归因于灰分通过影响电-热老化过程中PP的降解程度和结晶重排能力，最终导致灰分较高的BP-3熔融峰温度提升受限。灰分中的部分成分（如残留金属离子、未稳定的催化剂残渣等）可能成为氧化反应的催化剂，加速电-热老化中的自由基链式反应，降解产生的短链分子增多导致长程有序的晶体结构难以形成。低灰分薄膜BP-2中催化性杂质少，氧化降解更温和，分子链可保留更长的长度，仍具备较好的结晶重排能力，因此老化后晶体完善度提升更显著，熔融峰温度更高[17]。
此外，老化后BOPP薄膜的熔融峰均有变宽的趋势，这一现象可能来源于重结晶过程中新生成的部分次级有序结构。BOPP薄膜的结晶特性对其使用性能有着重要的影响，老化过程中BOPP薄膜结晶度和片晶厚度的增大，这主要源于薄膜受热时发生的重结晶现象。具体而言，无定形区中无规则排布的分子链段在热力学上处于不平衡的亚稳态，存在向稳定的热力学结构（结晶态）转变的趋势。因此在高温作用下，当非晶区分子链段获得足够的能量时，链段的运动单元得以在一定范围内发生移动和旋转，并向稳定的片晶结构转变，最终使得BOPP薄膜的片晶尺寸和宏观结晶度增大。
为了验证上述老化过程对薄膜分子链产生的降解作用，采用GPC进行进一步分析，老化前后样品的重均分子量如图8所示。从图8可以看出，老化后样品的重均分子量均有所减小，说明BOPP薄膜在老化过程中发生了分子链断裂。对于灰分含量较高的BP-3薄膜，其重均分子量下降了13.5%，洗涤低灰分BP-2薄膜分子量降幅仅为7.7%。这说明在电-热老化作用下，高灰分含量会促进薄膜分子链的断裂，进而影响了电-热老化前后薄膜的性能。
2.3　电学性能
对3种薄膜电容器老化1 000 h前后的电容值进行测试，评估其容量衰减和可靠性，结果如图9所示。从图9可以看出，老化前后BP-1制备的电容器FC-1容量从60.13 μF下降到59.93 μF，衰减率（ΔC）为0.33%。与之相比，FC-3电容器容量从60.17 μF下降到58.27 μF，衰减率高达3.16%；FC-2电容器容量从59.99 μF下降到58.94 μF，衰减率为1.75%。由此可见，FC-2电容器的容量保持率较FC-3电容器显著提升，但FC-2电容器的容量衰减较FC-1电容器仍然偏高，这可能是老化后薄膜分子量下降导致的。这说明灰分引起的载流子迁移和分子量下降可能是电容器容量衰减的主要原因。
为了进一步印证灰分对薄膜介电性能的影响，将电容器拆解后的薄膜在85℃、101～105 Hz下进行高温宽频介电测试，结果如图10所示，其中10 Hz下的对应数据如表4所示。从图10和表4可以看出，BP-1和BP-2薄膜老化前后，介电常数处于2.2～2.3，介质损耗因数小于0.003 5，二者随频率的升高均有小幅减小趋势。高灰分含量的BP-3薄膜老化后介电常数基本不变，但是在低频下的介质损耗因数超过0.005，且随频率的升高出现幅度较大的下降趋势。
对上述结果进行分析，聚丙烯作为一种非极性高聚物，其分子结构中不存在固有偶极矩。在低频外电场的激发作用下，该材料主要表现为界面极化，这种极化现象主要源于加工过程中引入的加工助剂、抗氧化剂以及部分小分子极性杂质等[18]。由于BP-1与BP-2薄膜的灰分含量相对较低，界面极化作用受到显著抑制，表现出介质损耗因数低于BP-3薄膜，且随频率变化的下降趋势更为平缓。在经历电-热老化处理后，高灰分薄膜BP-3在高温环境下分子链段发生断裂，同时载流子受到激发，导致其在低频条件下的载流子迁移弛豫效应显著增强，不仅介质损耗因数较高，且随频率升高呈现出显著的下降趋势。综上所述，灰分对薄膜的介电性能具有显著影响。低灰分国产树脂制备的BP-2薄膜具备更优异的高温介电性能，其性能已达到进口树脂制备的薄膜的同等水平。
灰分含量对薄膜的电气强度也会产生显著影响。图11为不同薄膜老化前后在85℃下的电气强度对比。从图11可以看出，3种薄膜老化后直流电气强度均呈现下降趋势，说明电-热老化会劣化其绝缘性能。其中高灰分薄膜BP-3老化后电气强度下降了8%，衰减最显著。从载流子迁移和结晶角度看，灰分的引入会增加载流子数量与迁移路径，电-热老化时，载流子迁移加剧，碰撞、积累易引发局部放电，损伤绝缘结构；同时，灰分的增多可能干扰BOPP薄膜的结晶规整性，使结晶缺陷增多，电场集中于缺陷处，加速绝缘破坏，致使其电气强度下降更明显[19]。相比之下，BP-1和BP-2薄膜的电气强度衰减幅度较小，绝缘性能更稳定。综上所述，通过降低树脂体系灰分的含量可以有效提升BOPP薄膜的绝缘性能以及工况下的性能稳定性。
3　结论
收起
本文系统研究了连续洗涤纯化国产低灰分聚丙烯树脂所制BOPP薄膜的理化性能、微观结构及80℃交-直流电-热联合老化行为，明确了灰分含量对薄膜结构与电学性能的调控机制，主要结论如下：
（1）灰分是影响BOPP薄膜表面形貌与结晶稳定性的关键因素，低灰分薄膜BP-1、BP-2表面“火山口”尺寸更小、分布更均匀；经电-热联合老化后，低灰分薄膜晶区结构无明显劣化，分子链降解程度显著低于高灰分薄膜BP-3。
（2）低灰分薄膜BP-2的高温介电性能与直流电气强度优异，85℃下的介电常数与介质损耗因数稳定，经80℃交-直流电-热联合老化1 000 h后，电容器容量衰减率与电气强度衰减幅度均远低于高灰分薄膜BP-3，可满足干式直流电容器的实际服役需求。

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2026年第59卷第7期
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doi: 10.16790/j.cnki.1009-9239.im.2026.07.010
  • 接收时间：2025-07-23
  • 首发时间：2026-09-10
  • 出版时间：2026-07-20
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  • 收稿日期：2025-07-23
  • 修回日期：2025-09-14
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    中国电力科学研究院有限公司 先进输电技术全国重点实验室，北京　102209

通讯作者:

邢照亮（1988-），男（汉族），山东临沂人，高级工程师，主要从事绝缘电介质材料的研究工作。
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2种不同金属材料的力学参数
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total species (%)		 属
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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
栓菌属 Trametes 5 2.39
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