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Article(id=1222482754743292731, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1222482747264852071, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.01.013, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1583164800000, receivedDateStr=2020-03-03, revisedDate=1591891200000, revisedDateStr=2020-06-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1769392201361, onlineDateStr=2026-01-26, pubDate=1611072000000, pubDateStr=2021-01-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1769392201361, onlineIssueDateStr=2026-01-26, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1769392201361, creator=13041195026, updateTime=1769392201361, updator=13041195026, issue=Issue{id=1222482747264852071, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='1', pageStart='1', pageEnd='107', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1769392199579, creator=13041195026, updateTime=1769414905563, updator=13041195026, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1222577983139861118, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1222482747264852071, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1222577983144055423, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1222482747264852071, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=73, endPage=77, ext={EN=ArticleExt(id=1222482755217249115, articleId=1222482754743292731, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Molecular Dynamics Simulation on Effect of Compound Curing Agent on Properties of Epoxy Resin System, columnId=1192878364340924664, journalTitle=Insulating Materials, columnName=Test and Analysis, runingTitle=null, highlight=null, articleAbstract=

In order to explore the effect of compound anhydride curing agent on the cured product of epoxy resin, we built crosslinking models of methyl tetrahydrophthalic anhydride (MTHPA)/phthalic anhydride (PA) (their compounding ratio was 10:0, 9:1, 7:3, 5:5, 0:10, respectively) and bisphenol A-type glycidyl ether (DGEBA) by molecular dynamics method. The effect of different compounding ratios on the structure, thermal properties, and mechanical properties of the crosslinking epoxy resin with the same crosslinking degree was studied. The results show that when the compounding ratio of MTHPA and PA is 10:0, the free volume proportion of system reaches maximum, and the motion ability of molecular chains is the strongest. When the compounding ratio is 7:3, the comprehensive mechanical properties of system reach the maximum. When the compounding ratio is 9:1 and 7:3, the glass transition temperature of system reaches the highest and the lowest, respectively.

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为探究复配酸酐固化剂对环氧树脂固化产物的影响，采用分子动力学方法建立了甲基四氢苯酐（MTHPA）/邻苯二甲酸酐（PA）（复配比分别为10∶0、9∶1、7∶3、5∶5、0∶10）和双酚A型缩水甘油醚（DGEBA）的交联模型，研究了在同一交联度下固化剂不同复配比对交联环氧树脂结构、热学性能和力学性能的影响。结果表明：当MTHPA和PA复配比为10∶0时，体系的自由体积占比最大，分子链段运动能力最强；复配比为7∶3时，体系的综合力学性能最好；而当复配比为9∶1时，体系的玻璃化转变温度最高，复配比为7∶3时最低。

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郝留成（1975-），男（汉族），河南平顶山人，教授级高级工程师，主要从事高电压绝缘技术的研究。

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郝留成（1975-），男（汉族），河南平顶山人，教授级高级工程师，主要从事高电压绝缘技术的研究。

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郝留成（1975-），男（汉族），河南平顶山人，教授级高级工程师，主要从事高电压绝缘技术的研究。

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体系复配比DGEBAMTHPAPA
110∶020400
29∶120364
37∶3202812
45∶5202020
50∶1020040
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不同体系模型分子数量

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体系复配比DGEBAMTHPAPA
110∶020400
29∶120364
37∶3202812
45∶5202020
50∶1020040
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体系占据体积/Å自由体积/Å自由体积占比/%
115 758.415 612.1526.26
215 709.414 791.6723.37
315 310.295 080.7524.92
415 111.384 476.2322.85
514 325.743 800.8520.97
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各体系自由体积计算

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体系占据体积/Å自由体积/Å自由体积占比/%
115 758.415 612.1526.26
215 709.414 791.6723.37
315 310.295 080.7524.92
415 111.384 476.2322.85
514 325.743 800.8520.97
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体系体积模量/GPa杨氏模量/GPa剪切模量/GPa
11.4172.5821.079
21.3843.0061.321
32.0263.7101.553
42.5363.4081.095
52.0703.4421.407
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不同体系的模量值

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体系体积模量/GPa杨氏模量/GPa剪切模量/GPa
11.4172.5821.079
21.3843.0061.321
32.0263.7101.553
42.5363.4081.095
52.0703.4421.407
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体系

玻璃化温度

/℃

拉伸强度

/MPa

弯曲强度

/MPa

冲击强度

/(kJ/m2)

11316512518
21586813412
31027914022
41328013919
51357913716
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不同体系的力学性能与热性能测试结果

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体系

玻璃化温度

/℃

拉伸强度

/MPa

弯曲强度

/MPa

冲击强度

/(kJ/m2)

11316512518
21586813412
31027914022
41328013919
51357913716
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复配固化剂对环氧树脂体系特性影响的分子动力学模拟
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郝留成 1 , 袁端鹏 1 , 陈蕊 1 , 张子扬 2 , 赵玉顺 2 , 谢庆 3 , 王波 4 , 宋忠孝 4
绝缘材料 | 测试与分析 2021,54(1): 73-77
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绝缘材料 | 测试与分析 2021, 54(1): 73-77
复配固化剂对环氧树脂体系特性影响的分子动力学模拟
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郝留成1, 袁端鹏1, 陈蕊1, 张子扬2, 赵玉顺2, 谢庆3, 王波4, 宋忠孝4
作者信息
  • 1平高集团有限公司 国家电网公司高压开关设备绝缘材料实验室，河南 平顶山 467001
  • 2合肥工业大学 电气与自动化工程学院，安徽 合肥 230009
  • 3华北电力大学 新能源电力系统国家重点实验室，河北 保定 071003
  • 4西安交通大学 金属材料强度国家重点实验室，陕西 西安 710049

    • 郝留成（1975-），男（汉族），河南平顶山人，教授级高级工程师，主要从事高电压绝缘技术的研究。

Molecular Dynamics Simulation on Effect of Compound Curing Agent on Properties of Epoxy Resin System
Liucheng HAO1, Duanpeng YUAN1, Rui CHEN1, Ziyang ZHANG2, Yushun ZHAO2, Qing XIE3, Bo WANG4, Zhongxiao SONG4
Affiliations
  • 1High Voltage Switchgear Insulating Materials Laboratory of State Grid, Pinggao Group Co., Ltd., Pingdingshan 467001, China
  • 2School of Electrical Engineering and Automation, Hefei University of Technology, Hefei 230009, China
  • 3State Key Laboratory of Alternate Electrical Power System with Renewable Energy Sources, North China Electric Power University, Baoding 071003, China
  • 4State Key Laboratory for Mechanical Behavior of Materials, Xi'an Jiaotong University, Xi'an 710049, China
出版时间: 2021-01-20 doi: 10.16790/j.cnki.1009-9239.im.2021.01.013
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为探究复配酸酐固化剂对环氧树脂固化产物的影响，采用分子动力学方法建立了甲基四氢苯酐（MTHPA）/邻苯二甲酸酐（PA）（复配比分别为10∶0、9∶1、7∶3、5∶5、0∶10）和双酚A型缩水甘油醚（DGEBA）的交联模型，研究了在同一交联度下固化剂不同复配比对交联环氧树脂结构、热学性能和力学性能的影响。结果表明：当MTHPA和PA复配比为10∶0时，体系的自由体积占比最大，分子链段运动能力最强；复配比为7∶3时，体系的综合力学性能最好；而当复配比为9∶1时，体系的玻璃化转变温度最高，复配比为7∶3时最低。

环氧树脂  /  酸酐固化剂  /  力学性能  /  玻璃化转变温度  /  分子模拟

In order to explore the effect of compound anhydride curing agent on the cured product of epoxy resin, we built crosslinking models of methyl tetrahydrophthalic anhydride (MTHPA)/phthalic anhydride (PA) (their compounding ratio was 10:0, 9:1, 7:3, 5:5, 0:10, respectively) and bisphenol A-type glycidyl ether (DGEBA) by molecular dynamics method. The effect of different compounding ratios on the structure, thermal properties, and mechanical properties of the crosslinking epoxy resin with the same crosslinking degree was studied. The results show that when the compounding ratio of MTHPA and PA is 10:0, the free volume proportion of system reaches maximum, and the motion ability of molecular chains is the strongest. When the compounding ratio is 7:3, the comprehensive mechanical properties of system reach the maximum. When the compounding ratio is 9:1 and 7:3, the glass transition temperature of system reaches the highest and the lowest, respectively.

epoxy resin  /  acid anhydride curing agent  /  mechanical properties  /  glass transition temperature  /  molecular simulation
郝留成, 袁端鹏, 陈蕊, 张子扬, 赵玉顺, 谢庆, 王波, 宋忠孝. 复配固化剂对环氧树脂体系特性影响的分子动力学模拟. 绝缘材料, 2021 , 54 (1) : 73 -77 . DOI: 10.16790/j.cnki.1009-9239.im.2021.01.013
Liucheng HAO, Duanpeng YUAN, Rui CHEN, Ziyang ZHANG, Yushun ZHAO, Qing XIE, Bo WANG, Zhongxiao SONG. Molecular Dynamics Simulation on Effect of Compound Curing Agent on Properties of Epoxy Resin System[J]. Insulating Materials, 2021 , 54 (1) : 73 -77 . DOI: 10.16790/j.cnki.1009-9239.im.2021.01.013
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0 引言
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环氧树脂作为电工绝缘材料，被广泛应用于输变电设备当中。随着电网向超高压、特高压输变电技术发展，对环氧绝缘材料的绝缘、耐老化和力学性能等提出了更为严苛的要求，研究设计满足上述优异性能的环氧树脂及其复合材料已经成为电网电工材料主流技术发展方向之一[1-3]。然而在传统的树脂材料设计中，由于环氧树脂和固化剂种类繁多和分子结构复杂，仅通过实验的方法设计并优化环氧树脂性能非常困难，并且具有研发周期长、效率低、成本高等缺点。随着计算机技术的发展，分子模拟为材料研发制备提供了新的设计思路，并且已被广泛用于预测和分析聚合物材料的性能，对实际应用有一定的指导作用，可以大幅节省时间与成本[4-9]。
本研究运用计算机分子模拟技术，构建甲基四氢苯酐（MTHPA）和邻苯二甲酸酐（PA）复配的固化剂与双酚A型缩水甘油醚（DGEBA）的交联环氧树脂体系模型，研究固化剂不同复配比对交联模型性能的影响，并对模拟结果进行试验验证。
1 交联模型的构建
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选用MTHPA和PA进行不同比例的复配研究，构建了5种聚合物的分子模型，其中环氧树脂分子选用DGEBA，MTHPA和PA复配比分别为10∶0、9∶1、7∶3、5∶5、0∶10，模型中分子数量如表1所示。
模型构建步骤如下：
（1）分别构建并优化MTHPA、PA和DGEBA单体分子模型，如图1所示。再利用Amorphous Cell模块建立表1中设定的5种分子模型结构，设定初始密度为0.9 g/cm3。
（2）对上步构建的分子模型取最后一帧进行分子动力学几何优化，获得优化后的分子结构再次进行分子动力学模拟，步骤如下：先在NVT系综下进行100 ps分子动力学模拟，使得分子链得到进一步松弛；然后在NPT系综下进行200 ps分子动力学模拟以获得更加合理的体系密度。两次模拟温度均设为298 K，步长为1 fs，压强为0.1 MPa，力场为COMPASS，控温方法采用Andersen[10]，控压方法采用Berendsen[11]。
（3）模拟环氧树脂与固化剂的交联过程，依据环氧树脂与酸酐固化剂的反应原理，编制基于Perl语言的交联程序以实现环氧树脂体系的固化交联[12-13]。设定初始截断半径为3.5 Å，最大截断半径为10 Å，步长为0.5 Å，反应温度为600 K。最终得到5个体系的交联分子模型，如图2所示（选取90%的交联度）。
2 结果与讨论
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2.1 自由体积
环氧树脂交联结构的自由体积与其性能存在一定关联性。当交联结构由橡胶态转变为玻璃态时，体系的自由体积减小，会阻碍交联结构中分子链段的运动，同时较小的自由体积也可以有效地阻碍小分子物质在交联结构中扩散。自由体积的大小影响着聚合物体系的玻璃化转变温度、模量等参数。
由于不同体系中总体积Vt（包括自由体积Vf和分子占据体积V0）不同，为能够更加直观地显示各体系的自由体积差异，使用自由体积占比（FFV）来进行分析。FFV表示自由体积的相对大小，其计算公式如式（1）所示。
FFV=VfV0+Vf
各个体系的自由体积计算结果如表2所示。从表2可以看出，随着PA用量增加，体系自由体积占比总体呈下降趋势，当固化剂分子全为PA时，自由体积占比最低，为20.97%。这是因为与PA分子相比，MTHPA分子化学结构中有甲基类侧基，侧基的存在使分子间距离增大，自由体积相对较大。
2.2 均方位移
分子动力学模拟可以计算系统各种动态的特性，反映出系统中粒子的运动状态，可借此了解各种形态的运动。动力学模拟过程中体系内原子自起始位置不停移动，在每一瞬间各原子的位置皆不相同，粒子位移平方的平均值称为MSD，可用于描述高分子链段的运动能力，其计算公式为式（2）。
MSD=13N∑i=0N-1Rit-Ri(0)2
式（2）中：Ri(0)和Ri(t)分别为系统中任一原子i在初始时间和t时刻的位移矢量；N为计算系统内的原子总数。
图3为5个体系在298 K温度下进行40 ps后的MSD图。从图3可以看出，随着时间的增加，分子链段的移动距离不断增大，并且MSD值由大到小依次为体系1、3、2、4、5，这与表2中FFV的大小顺序对应。说明交联体系中的自由体积占比越大，体系内部相对自由体积越大，分子链段的运动能力越强。
2.3 力学性能
在分子模拟中，可以通过静态分析方法来获得系统的力学性能，即在已经达到力学平衡的体系中施加一个微小的应变，通过对发生微小形变模型进行内力和应变分析计算得到材料的刚度矩阵和Lame常数λ、μ[14]。由Lame常数可进一步得到体系的体积模量K、杨氏模量E、剪切模量G等力学性能参数。计算得到5种体系的体积模量、杨氏模量和剪切模量如表3所示。从表3可以看出，体系3的杨氏模量和剪切模量最大，体积模量仅次于体系4，综合来看其力学性能最好。从表3还可以看出，体系3、4、5的模量值均大于体系1，说明PA的加入有助于提升交联环氧树脂的力学性能，其中当MTHPA和PA的复配比为7∶3时提升最明显。究其原因在于，PA的加入有利于体系形成致密的交联结构，增强了材料的物理缠结作用，在进行拉伸与弯曲时，产生应力分散和应力承受作用，达到了增强固化物韧性的作用。
2.4 热学性能
随着温度的升高，材料的体积和密度会有一定的变化，利用环氧树脂交联体系在玻璃态和橡胶态性能差异很大这一特性，可以分别计算多个温度下的体系密度，对温度-密度曲线分段进行线性拟合，两条拟合直线的交点对应的温度即为该体系的玻璃化转变温度（Tg）[15]。
分别对建立的交联体系进行300～600 K的退火模拟，降温速率为50 K/300 ps，取体系每个温度下最后100 ps的密度平均值，视为该温度下的密度值。根据上述方法得到各个体系的温度-密度图及Tg如图4所示。从图4可以看出，体系1～5的Tg分别为455、486、390、426、431 K。当MTHPA和PA的复配比为9∶1时，交联环氧树脂的Tg最高，高于纯MTHPA和纯PA交联体系。说明采用MTHPA和PA混合型固化剂的配方，可以提高固化物的交联程度，形成高度交联的结构，从而使体系具有高耐热性能。但当MTHPA和PA复配比为7∶3时，Tg为390 K，是5个体系中最低的。因此，选择合适的固化剂配比可以提高环氧树脂的Tg。
3 试验验证
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为了验证分子模型模拟热学与力学性能的可靠性，针对5种配方体系进行材料性能试验验证，主要进行玻璃化温度、拉伸强度、弯曲强度、冲击强度测试，并将所得实际测试结果与分子模拟结果做对比。
试样制备流程：首先将DGEBA、MTHPA和PA分别在烘箱中50℃下预热60 min，将预热好的DGEBA转移至在小型浇注设备混料罐中，在50℃下抽真空处理30 min。然后将MTHPA和PA两种固化剂按比例混合均匀后加入DGEBA中，在50℃下搅拌并抽真空处理10 min，使3种料混合均匀并去除气泡后，将其浇注至涂有涂膜剂并预热好的模具中。随后放入烘箱在100℃固化3 h，脱模后在130℃下固化12 h，最终获得拉伸样条、弯曲样条、冲击样条和热性能测试试样。
体系1～5的玻璃化温度、拉伸强度、弯曲强度、冲击强度测试结果如表4所示。从表4可以看出，体系2的玻璃化转变温度最高，体系3的综合力学性能最好，与分子模拟结果相吻合，证明了MTHPA/PA与环氧树脂交联模型的可靠性。
4 结论
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（1）当固化剂分子为MTHPA时，自由体积占比最大，分子链段运动能力最强，随着PA的增加，交联体系自由体积占比减小，分子链段能力减弱。
（2）当固化剂MTHPA与PA的复配比为7∶3时，交联体系的综合力学性能最好。
（3）当MTHPA和PA配比为9∶1时，交联环氧树脂的Tg最高，选择合适的复配比可有效提高环氧树脂的Tg。
基金
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  • 国家重点研发计划项目(2017YFB0903800)
  • 国家重点研发计划项目(2017YFB0903803)
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2021年第54卷第1期
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文章信息
doi: 10.16790/j.cnki.1009-9239.im.2021.01.013
  • 接收时间：2020-03-03
  • 首发时间：2026-01-26
  • 出版时间：2021-01-20
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  • 收稿日期：2020-03-03
  • 修回日期：2020-06-12
基金
国家重点研发计划项目(2017YFB0903800)
国家重点研发计划项目(2017YFB0903803)
作者信息
    1平高集团有限公司 国家电网公司高压开关设备绝缘材料实验室，河南 平顶山 467001
    2合肥工业大学 电气与自动化工程学院，安徽 合肥 230009
    3华北电力大学 新能源电力系统国家重点实验室，河北 保定 071003
    4西安交通大学 金属材料强度国家重点实验室，陕西 西安 710049
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2种不同金属材料的力学参数
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
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