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Article(id=1203281642178719971, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.06.008, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1720713600000, receivedDateStr=2024-07-12, revisedDate=1725465600000, revisedDateStr=2024-09-05, acceptedDate=null, acceptedDateStr=null, onlineDate=1764814299387, onlineDateStr=2025-12-04, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764814299387, onlineIssueDateStr=2025-12-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764814299387, creator=13701087609, updateTime=1764814299387, updator=13701087609, issue=Issue{id=1203281635908231645, tenantId=1146029695717560320, journalId=1149653034449285133, year='2025', volume='58', issue='6', pageStart='1', pageEnd='148', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1764814297892, creator=13701087609, updateTime=1764815002353, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1203284590690545746, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1203284590694740051, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=61, endPage=66, ext={EN=ArticleExt(id=1203281642518458608, articleId=1203281642178719971, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Modification and research of DOPO-based oligomer flame retardant for bisphenol A epoxy resin, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=

Bisphenol A epoxy resin is widely used in the field of copper clad laminates. However, its flame retardancy and dielectric properties cannot meet the high-speed development of copper clad laminates. To simultaneously improve the flame retardancy and dielectric properties of epoxy resin, a reactive oligomeric flame retardant (PDDV) based on 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ), 1,4-dichlorobenzene (DCX), and 4-vinylbenzyl chloride (VBC) was synthesized, and its chemical structure was determined by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) characterization. EP/PDDV composites were prepared by physical blending, and their thermal, flame retardancy, and dielectric properties were tested. The results show that when the mass fraction of PDDV is 30%, the char yield of EP/PDDV composites increases to 38.74%, the glass transition temperature (Tg) rises to 138.9℃, the limiting oxygen index (LOI) increases to 55%, UL-94 reaches V-0 grade, the dielectric constant (Dk) is 2.69, and the dielectric loss factor (Df) is 0.007 91. The comprehensive performance of the composites is the best.

, articleAbstract=

Bisphenol A epoxy resin is widely used in the field of copper clad laminates. However, its flame retardancy and dielectric properties cannot meet the high-speed development of copper clad laminates. To simultaneously improve the flame retardancy and dielectric properties of epoxy resin, a reactive oligomeric flame retardant (PDDV) based on 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ), 1,4-dichlorobenzene (DCX), and 4-vinylbenzyl chloride (VBC) was synthesized, and its chemical structure was determined by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) characterization. EP/PDDV composites were prepared by physical blending, and their thermal, flame retardancy, and dielectric properties were tested. The results show that when the mass fraction of PDDV is 30%, the char yield of EP/PDDV composites increases to 38.74%, the glass transition temperature (Tg) rises to 138.9℃, the limiting oxygen index (LOI) increases to 55%, UL-94 reaches V-0 grade, the dielectric constant (Dk) is 2.69, and the dielectric loss factor (Df) is 0.007 91. The comprehensive performance of the composites is the best.

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双酚A型环氧树脂被广泛应用于覆铜板领域，然而其阻燃性能和介电性能无法满足覆铜板高速化的发展。为同时提高环氧树脂的阻燃性能和介电性能，合成了一种基于10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO-HQ）、1,4-对二氯苄（DCX）和4-乙烯基苄氯（VBC）的反应型低聚物阻燃剂（PDDV）。通过红外光谱分析（FTIR）、核磁表征（NMR）确定了PDDV的化学结构。通过物理共混制备了EP/PDDV复合材料，并对其热学性能、阻燃性能及介电性能进行测试。结果表明：当PDDV的质量分数为30%时，EP/PDDV复合材料的残炭率提高至38.74%，玻璃化转变温度（Tg）上升至138.9℃，极限氧指数（LOI）提高到了55.0%，UL-94达到V-0等级，介电常数（Dk）为2.69，介质损耗因数（Df）为0.007 91，表明该复合材料的综合性能最佳。

, articleAbstract=

双酚A型环氧树脂被广泛应用于覆铜板领域，然而其阻燃性能和介电性能无法满足覆铜板高速化的发展。为同时提高环氧树脂的阻燃性能和介电性能，合成了一种基于10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO-HQ）、1,4-对二氯苄（DCX）和4-乙烯基苄氯（VBC）的反应型低聚物阻燃剂（PDDV）。通过红外光谱分析（FTIR）、核磁表征（NMR）确定了PDDV的化学结构。通过物理共混制备了EP/PDDV复合材料，并对其热学性能、阻燃性能及介电性能进行测试。结果表明：当PDDV的质量分数为30%时，EP/PDDV复合材料的残炭率提高至38.74%，玻璃化转变温度（Tg）上升至138.9℃，极限氧指数（LOI）提高到了55.0%，UL-94达到V-0等级，介电常数（Dk）为2.69，介质损耗因数（Df）为0.007 91，表明该复合材料的综合性能最佳。

, correspAuthors=null, authorNote=null, correspAuthorsNote=
唐安斌（1968-），男（汉族），四川南充人，研究员，博士，主要从事新型绝缘材料、光学显示材料、先进电子材料及环保阻燃材料的研究。
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李昕宇（2000-），男（汉族），四川南充人，硕士生，主要从事低介质损耗含磷阻燃剂的研究；

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李昕宇（2000-），男（汉族），四川南充人，硕士生，主要从事低介质损耗含磷阻燃剂的研究；

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李昕宇（2000-），男（汉族），四川南充人，硕士生，主要从事低介质损耗含磷阻燃剂的研究；

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试样编号D128/gDFE618/gPDDV
质量/g质量分数/%
EP-05061.2500
EP-205061.2512.520
EP-255061.2516.6525
EP-305061.2521.4530
EP-355061.2526.9035
EP-405061.2533.3540
), ArticleFig(id=1203362952532439209, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281642178719971, language=CN, label=表1, caption=

EP/PDDV复合材料的配方

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试样编号D128/gDFE618/gPDDV
质量/g质量分数/%
EP-05061.2500
EP-205061.2512.520
EP-255061.2516.6525
EP-305061.2521.4530
EP-355061.2526.9035
EP-405061.2533.3540
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GPCMn/(g/mol)Mw/(g/mol)Mz/(g/mol)Mz/MwMw/Mn占比/%
Peak11 8351 8391 8431.0021.00232.393
Peak21 4171 4231 4281.0041.00449.670
Peak31 0071 0111 0141.0031.0039.159
Peak45755795841.0071.0078.778
Total1 4411 4461 4501.0031.004100
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PDDV的GPC

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GPCMn/(g/mol)Mw/(g/mol)Mz/(g/mol)Mz/MwMw/Mn占比/%
Peak11 8351 8391 8431.0021.00232.393
Peak21 4171 4231 4281.0041.00449.670
Peak31 0071 0111 0141.0031.0039.159
Peak45755795841.0071.0078.778
Total1 4411 4461 4501.0031.004100
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试样编号LOI/%UL-94
t1/st2/s是否滴落等级
EP-024.5>30—否NR
EP-2046.216.912.7否V-1
EP-2547.613.28.1否V-1
EP-3055.03.52.1否V-0
EP-3549.311.64.2否V-1
EP-4048.912.56.4否V-1
), ArticleFig(id=1203362952972841155, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281642178719971, language=CN, label=表3, caption=

EP/PDDV复合材料的阻燃性能

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试样编号LOI/%UL-94
t1/st2/s是否滴落等级
EP-024.5>30—否NR
EP-2046.216.912.7否V-1
EP-2547.613.28.1否V-1
EP-3055.03.52.1否V-0
EP-3549.311.64.2否V-1
EP-4048.912.56.4否V-1
), ArticleFig(id=1203362953069310155, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281642178719971, language=EN, label=Table 4, caption=The dielectric properties of EP/PDDV composite, figureFileSmall=null, figureFileBig=null, tableContent=
试样编号Dk (10 GHz)Df (10 GHz)
EP-03.820.018 07
EP-202.950.008 61
EP-252.810.008 08
EP-302.690.007 91
EP-352.530.007 39
EP-402.410.006 94
), ArticleFig(id=1203362953153196239, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281642178719971, language=CN, label=表4, caption=

EP/PDDV复合材料的介电性能

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试样编号Dk (10 GHz)Df (10 GHz)
EP-03.820.018 07
EP-202.950.008 61
EP-252.810.008 08
EP-302.690.007 91
EP-352.530.007 39
EP-402.410.006 94
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DOPO基低聚物阻燃剂对双酚A型环氧树脂的改性与研究
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李昕宇 1, 2 , 周友 3 , 唐安斌 1, 3
绝缘材料 | 材料研究 2025,58(6): 61-66
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绝缘材料 | 材料研究 2025, 58(6): 61-66
DOPO基低聚物阻燃剂对双酚A型环氧树脂的改性与研究
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李昕宇1, 2, 周友3, 唐安斌1, 3
作者信息
  • 1.中国科学院 成都有机化学研究所，四川 成都 610213
  • 2.中国科学院大学，北京 100190
  • 3.四川东材科技集团股份有限公司，四川 绵阳 621000

    • 李昕宇（2000-），男（汉族），四川南充人，硕士生，主要从事低介质损耗含磷阻燃剂的研究；

通讯作者:

唐安斌（1968-），男（汉族），四川南充人，研究员，博士，主要从事新型绝缘材料、光学显示材料、先进电子材料及环保阻燃材料的研究。
Modification and research of DOPO-based oligomer flame retardant for bisphenol A epoxy resin
Xinyu LI1, 2, You ZHOU3, Anbin TANG1, 3
Affiliations
  • 1. Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610213, China
  • 2. University of Chinese Academy of Sciences, Beijing 100190, China
  • 3. Sichuan EM Technology Co., Ltd., Mianyang 621000, China
出版时间: 2025-06-20 doi: 10.16790/j.cnki.1009-9239.im.2025.06.008
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摘要
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双酚A型环氧树脂被广泛应用于覆铜板领域，然而其阻燃性能和介电性能无法满足覆铜板高速化的发展。为同时提高环氧树脂的阻燃性能和介电性能，合成了一种基于10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO-HQ）、1,4-对二氯苄（DCX）和4-乙烯基苄氯（VBC）的反应型低聚物阻燃剂（PDDV）。通过红外光谱分析（FTIR）、核磁表征（NMR）确定了PDDV的化学结构。通过物理共混制备了EP/PDDV复合材料，并对其热学性能、阻燃性能及介电性能进行测试。结果表明：当PDDV的质量分数为30%时，EP/PDDV复合材料的残炭率提高至38.74%，玻璃化转变温度（Tg）上升至138.9℃，极限氧指数（LOI）提高到了55.0%，UL-94达到V-0等级，介电常数（Dk）为2.69，介质损耗因数（Df）为0.007 91，表明该复合材料的综合性能最佳。

环氧树脂  /  低聚物阻燃剂  /  低介质损耗  /  热性能  /  覆铜板

Bisphenol A epoxy resin is widely used in the field of copper clad laminates. However, its flame retardancy and dielectric properties cannot meet the high-speed development of copper clad laminates. To simultaneously improve the flame retardancy and dielectric properties of epoxy resin, a reactive oligomeric flame retardant (PDDV) based on 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-HQ), 1,4-dichlorobenzene (DCX), and 4-vinylbenzyl chloride (VBC) was synthesized, and its chemical structure was determined by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) characterization. EP/PDDV composites were prepared by physical blending, and their thermal, flame retardancy, and dielectric properties were tested. The results show that when the mass fraction of PDDV is 30%, the char yield of EP/PDDV composites increases to 38.74%, the glass transition temperature (Tg) rises to 138.9℃, the limiting oxygen index (LOI) increases to 55%, UL-94 reaches V-0 grade, the dielectric constant (Dk) is 2.69, and the dielectric loss factor (Df) is 0.007 91. The comprehensive performance of the composites is the best.

epoxy resin  /  oligomeric flame retardant  /  low dielectric loss  /  thermal performance  /  copper clad laminates
李昕宇, 周友, 唐安斌. DOPO基低聚物阻燃剂对双酚A型环氧树脂的改性与研究. 绝缘材料, 2025 , 58 (6) : 61 -66 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.008
Xinyu LI, You ZHOU, Anbin TANG. Modification and research of DOPO-based oligomer flame retardant for bisphenol A epoxy resin[J]. Insulating Materials, 2025 , 58 (6) : 61 -66 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.008
正文
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0 引言
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环氧树脂（EP）具有质量轻、耐腐蚀、易加工以及绝缘性能优异等特点，被广泛应用于涂料、粘合剂、印刷电路板以及电子绝缘材料等领域[1-2]，是制备覆铜板（CCL）理想的基体树脂之一。随着集成电路行业的快速发展，高速CCL逐渐成为印刷电路板领域的主要研究方向[3]。为了提高信号传输速率、增大数据传输容量、降低通信延迟，并且保证电路的使用安全，对所有承载信号传输、转换和记录功能的电子器件载体提出了更高的要求[4-5]。然而由于EP具有耐热性差、易燃烧的缺点[6]，并且EP中环氧基等极性官能团的偶极极化会增大材料的介电常数（Dk）和介质损耗因数（Df）[7]，进而影响高速CCL的信号传输。因此，要实现EP在高速CCL领域的广泛应用，需使其同时具有优异的阻燃性能和更低的介质损耗。
向EP中添加阻燃剂是提升其阻燃性能最便捷的方法[8]。磷系阻燃剂由于具有较高的阻燃效率并且绿色无污染[9]，被广泛应用于EP的阻燃改性。目前，红磷、聚磷酸铵（APP）、磷酸盐等添加型无机磷系阻燃剂在市场上的应用最为广泛[10]，但此类非聚合型阻燃剂在使用过程中需大量添加，且存在与聚合物基体相容性差、易迁移析出等缺点[11]。而聚合型阻燃剂能有效提高阻燃剂与基体的相容性，使其在加工及使用过程中不易迁移[12]。10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO-HQ）作为一种新型的含磷阻燃剂，其两端的羟基可以与其他活性官能团反应制备聚合型含磷阻燃剂[13]。因此，通过引入双键等活性基团，可以使阻燃剂分子具有一定的反应活性，此外还可以引入一些具有较大空间位阻的非极性官能团，赋予阻燃剂良好的介电性能，从而达到改善EP复合材料介电性能的目的。
本研究以DOPO-HQ和1,4-对二氯苄（DCX）为原料，4-乙烯基苄氯（VBC）为封端剂，合成了一种聚合型低介质损耗含磷阻燃剂（PDDV），并将其与双酚A型环氧树脂共混制备EP/PDDV复合材料。详细表征EP/PDDV复合材料的热学性能和介电性能，并结合PDDV分子结构特点，探究其阻燃性能和介电性能提高的机理。
1 实验部分
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1.1 主要原材料
双酚A型环氧树脂（D128）、活性酯固化剂（DFE618），工业级，四川东材科技集团股份有限公司；10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO-HQ），分析纯，江阴市涵丰科技有限公司；1,4-对二氯苄（DCX），电子级，青岛和兴精细化学有限公司；4-乙烯基苄氯（VBC），分析纯，山东星顺新材料有限公司；氢氧化钠（NaOH）、丁酮（MEK）、异丙醇，分析纯，成都市科隆化学品有限公司；N,N-二甲基甲酰胺（DMF），分析纯，成都金山化学试剂有限公司；玻璃纤维布，电子级，市售；铜箔，电解铜，市售。
1.2 PDDV的合成
在氮气氛围下，将48.6 g（0.15 mol）DOPO-HQ分散于300 mL DMF中，将其加入配备有机械搅拌器、冷凝管和温控装置的500 mL四颈圆底烧瓶中，在79℃下搅拌30 min至溶液无色澄清。然后将16 g（0.4 mol）NaOH加入混合溶液中，搅拌1 h至溶液呈红褐色。随后向烧瓶中加入17.5 g（0.1 mol）DCX，继续搅拌8 h。之后向体系中添加15.25 g（0.1 mol）VBC，在69℃下反应6 h。反应结束后，将红褐色溶液通过真空抽滤得到棕色溶液，并将棕色溶液逐滴加入大量异丙醇中，不断搅拌，直至析出粉白色絮状聚合物，将产物置于70℃真空烘箱内干燥12 h。最后用去离子水洗涤聚合物3次，过滤烘干研磨后得到最终固体产物（PDDV）。具体合成路线如图1所示。
1.3 EP/PDDV复合材料的制备
胶液制备：按一定比例将PDDV添加到D128中，在80℃下搅拌30 min，直至烧杯内液体变为均相，再向其中加入一定化学计量的固化剂DFE618，在60℃下减压搅拌至溶液无气泡产生，随后向溶液中加入一定量的溶剂MEK配置成固含量为65%的胶液。EP/PDDV复合材料的配方见表1。
半固化片的制备：将玻璃纤维布浸渍于上述胶液中，均匀上胶后放入140℃烘箱中预固化1 h，制得半固化片备用。
层压板的制备：将20张半固化片叠配，上下两面均覆盖一层铜箔，然后在两侧加钢板和缓冲牛皮纸并放入真空压机。设定高温真空热压机程序（160℃/30 min+210℃/90 min），加压并保持一定真空度，压合制得EP/PDDV层压板。
1.4 测试与表征
红外光谱（FTIR）：采用美国Perkin Elmer公司生产的Spectrum Two型傅里叶变换红外光谱仪进行测试，使用KBr压片法，波数为400～4 000 cm-1。
凝胶渗透色谱（GPC）：采用日本东曹公司生产的HLC-8420GPC型色谱仪进行测试，四氢呋喃（THF）为溶剂，流速为1.0 mL/min。
核磁共振（NMR）：采用德国Bruker公司生产的FX201502型核磁共振波谱仪进行测试，二甲基亚砜（DMSO）为溶剂，测试频率为600 MHz。
差示扫描量热（DSC）：采用德国Netzsch公司生产的DSC200F3型差示扫描量热仪进行测试，氮气氛围，升温速率为10℃/min，测试温度为室温～250℃。
热重分析（TGA）：采用德国Netzsch公司生产的TG209F3 Tarsus型热失重分析仪进行测试，氮气氛围，升温速率为10℃/min，测试温度为室温～600℃。
极限氧指数（LOI）：采用英国Stanton Redcroft公司生产的31D-38型氧指数测定仪，根据GB/T 2406.2—2009进行测试，样品尺寸为80 mm×6 mm×3 mm。
垂直燃烧（UL-94）：采用昆山阳屹测试仪器仪表有限公司生产的5402-A1型垂直燃烧仪，根据ASTM D 3801进行测试，样品尺寸为130 mm×13 mm×3 mm。
介电性能：采用美国Keysight公司生产的P9373A型网络分析仪和波兰QWED公司生产的SPDR夹具，根据GB/T 9534—1988进行测试，测试频率为10 GHz。
2 结果与讨论
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2.1 PDDV的结构表征与热学性能分析
2.1.1 红外分析
采用红外光谱（FTIR）对PDDV和DOPO-HQ的结构进行表征，结果如图2所示。从图2可以看出，DOPO-HQ中的特征峰1 583 cm-1（P-Ph）、1 197 cm-1（P=O）、923 cm-1（P-O-Ph）在PDDV的FTIR谱图中均得以保留。在PDDV的FTIR谱图中于1 665 cm-1和1 152 cm-1处出现两个新的吸收峰，它们分别对应于C=C以及C-O-C结构，并且DOPO-HQ中3 406 cm-1（-OH）处的特征峰在PDDV谱图中消失，表明PDDV被成功合成。
2.1.2 核磁分析
图3为PDDV的1H NMR谱图，具体结构如下，a,b：-CH2-O（5.03～5.16）、c：=CH2（5.20～5.41）、d：=CH2（5.64～5.97）、e：=CH（6.63～7.05）、f～q：C-Ph（7.07～8.15）。分子中所有的氢原子均可根据裂分原理及化学位移影响因素进行归属，进一步确定了PDDV的化学结构。
2.1.3 凝胶渗透色谱分析
凝胶渗透色谱是测定聚合物分子量及其分布的重要方法之一[14]，PDDV的GPC结果如表2所示。从表2可以看，PDDV的数均分子量（Mn）为1 441 g/mol，重均分子量（Mw）为1 446 g/mol，多分散系数（Mw/Mn）为1.004，分子量分布均匀，表明成功合成了聚合度为2～3的低聚物，符合设计所需分子量要求。
2.1.4 热学性能分析
热重分析是检测材料热分解性能最常用的方法之一[15]。PDDV在氮气中的TGA和DTG曲线如图4所示。从图4可以看出，PDDV的热解过程分为3个阶段，第1个阶段为142.6～248.5℃，主要是PDDV分子两端双键活性基团交联形成的网络结构断裂导致失重，其中质量损失5%的温度（T5%）为195.4℃。第2阶段为261.8～339.7℃，主要是由于醚键的热裂解和部分低分子量的PDDV的早期热分解，产生DOPO基链段，导致失重。而主要降解阶段发生在377.9～583.8℃（第3阶段），这一阶段聚合物主链断裂，DOPO基链段在氮气环境中主要分解为二苯并呋喃、PO·和PO2·[16]，最大质量损失速率的温度（Tmax）为500.2℃，在600℃时的残炭率高达44.88%。
2.2 EP/PDDV复合材料的热学性能分析
图5为EP/PDDV复合材料在氮气氛围中的TGA和DTG曲线。
从图5(a)可以看出，各组EP/PDDV复合材料的T5%均高于纯EP，这主要是因为在燃烧过程中DOPO会受热分解形成致密的保温层，提高了复合材料的热稳定性[17]；此外各组EP/PDDV复合材料燃烧后的残炭率均高于纯EP的残炭率20.32%，其中EP-30残炭率达到最大值38.74%，结合PDDV的自成炭性可得出磷氧基团以及聚苯甲醚结构的引入提高了树脂材料的阻燃性能，但体系中过高的阻燃剂含量同样会降低聚合物在高温下的残炭率。从图5(b)可以看出，各组EP/PDDV复合材料均只有1个分解台阶，Tmax均高于纯EP的Tmax 412.3℃，进一步说明复合材料的热稳定性得到提高。
玻璃化转变温度（Tg）是评估EP热稳定性的另一个重要参数，各组EP/PDDV复合材料的DSC曲线如图6所示。从图6可以看出，纯EP的Tg值为90.3℃，当PDDV的质量分数为30%时，样品EP-30的Tg值升高到138.9℃，当PDDV的质量分数为35%时，样品EP-35的Tg值达到最大值146.4℃，这是由于PDDV分子两端含有双键官能团，反应活性较高，易发生自交联反应，形成较大的交联网络，从而提高体系交联密度，其中含有的苯环等刚性结构，也限制了环氧树脂分子链的运动[18]。当PDDV的质量分数达到40%时，由于过量PDDV的聚集，样品EP-40的Tg值略有下降。
2.3 EP/PDDV复合材料的阻燃性分析
极限氧指数（LOI）和垂直燃烧测试（UL-94）被广泛应用于评价材料的阻燃性能。EP/PDDV复合材料的LOI和UL-94测试结果如表3所示。
从表3可以看出，样品EP-0在点燃后迅速燃烧。当阻燃剂PDDV的质量分数为30%时，样品EP-30的LOI可达到55.0%，属于难燃材料[19]，且通过UL-94测试的V-0等级。
样品EP-0在UL-94垂直燃烧测试中剧烈燃烧，无法自熄，而样品EP-30则在10 s内自熄，说明PDDV的引入提高了EP的阻燃性能，这主要归因于3个方面：①DOPO结构受热分解产生的PO·和PO2·通过捕捉燃烧时气相中产生的HO·和H·来抑制燃烧过程中的链式反应从而中断燃烧；②PDDV的加入促进了环氧树脂基体表面的初始催化成炭作用[20]；③DOPO基团在燃烧过程中产生的大量的不可燃烧气体如CO2、H2O可以稀释氧气，进一步抑制聚合物材料的燃烧。然而添加过量的PDDV会导致复合材料的LOI值降低以及UL-94等级下降，这主要是由于过量的PDDV发生团聚，使EP/PDDV复合材料在燃烧过程中的降解速率大于成炭速率。
2.4 EP/PDDV复合材料的介电性能分析
介电性能是影响覆铜板信号传输速率和传输效率的重要因素之一[21]。Dk和Df低的基板在高频信号传输过程中可以更好地达到高保真、低延迟的效果[22]。EP/PDDV复合材料在10 GHz频率下的Dk和Df如表4所示。从表4可以看出，相较于纯EP，EP/PDDV复合材料的Dk和Df均有明显的下降，并呈现出线性减小的趋势，当PDDV的质量分数为40%时，样品EP-40的Dk为2.41，Df为0.006 94。通常可通过降低材料极性、增大材料中自由体积分数等方法来减小材料的介电常数[23]。PDDV分子链结构对称性好，本身是一种低介电材料，同时PDDV中含有大量苯环等非极性基团，将其引入环氧树脂中，在降低材料极性的同时还增大了固化体系的自由体积分数，使得复合材料的介电常数降低。
3 结论
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本文成功合成了一种基于DOPO-HQ、DCX和VBC的聚合型低介质损耗阻燃剂（PDDV），并将其作为反应型阻燃剂应用于EP中。从DSC和TGA结果可以看出，PDDV能有效提高环氧树脂的Tg和残炭率。在燃烧测试中，EP-30的LOI值可提高到55.0%，并通过了UL-94测试的V-0等级。介电性能测试数据表明，PDDV的加入有效降低了EP的Dk和Df，其中EP-40的Dk达到最小值2.41，Df为0.006 94，表现出优异的介电性能。综合纯EP材料以及各组EP/PDDV复合材料的阻燃性能和介电性能，当PDDV的质量分数为30%时，EP/PDDV复合材料的综合性能最佳。
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2025年第58卷第6期
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doi: 10.16790/j.cnki.1009-9239.im.2025.06.008
  • 接收时间：2024-07-12
  • 首发时间：2025-12-04
  • 出版时间：2025-06-20
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  • 收稿日期：2024-07-12
  • 修回日期：2024-09-05
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    1.中国科学院 成都有机化学研究所，四川 成都 610213
    2.中国科学院大学，北京 100190
    3.四川东材科技集团股份有限公司，四川 绵阳 621000

通讯作者:

唐安斌（1968-），男（汉族），四川南充人，研究员，博士，主要从事新型绝缘材料、光学显示材料、先进电子材料及环保阻燃材料的研究。
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
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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