摘要
用格氏法制备了苯乙炔封端的含硅芳炔树脂(FEC-PSA),采用核磁共振氢谱、红外光谱、凝胶渗透色谱、粘度测试、示差扫描量热分析及热重分析对该树脂的固化反应和流变性能以及三种镍系催化剂和三种钴系催化剂对FEC-PSA树脂的固化反应和固化物热稳定性的影响进行了研究。结果表明,FEC-PSA树脂的加工性能好,其加工窗口可达140℃,90℃下树脂粘度低于50 mPa·s,但其起始固化温度高于290℃。加入催化剂可显著降低FEC-PSA的固化温度。与高温热固化的FEC-PSA相比,双(三苯基膦)二羰基镍可分别降低FEC-PSA的起始固化温度(T_(i))和峰值温度(T_(p))约70℃和100℃,固化树脂的5%热失重温度(T_(d5))和800℃残炭率(Y_(r800℃))可分别提高至537℃和87%。二茂钴可降低FEC-PSA的T_(i)和T_(p)约70℃以上,而固化树脂的T_(d5)和Y_(r800℃)可分别提高至495℃和86%。
The silicon-containing polyarylacetylene(PSA) was prepared and fully end-capped(FEC)with phenylacetylene according to Grignard process. The cure reaction and rheological behavior of FEC-PSA resin and the effects of three nickel-based catalysts and three cobalt-based catalysts on the curing reaction of the FEC-PSA resin and the thermal stability of the cured FEC-PSA resin were studied by hydrogen nuclear magnetic resonance spectroscopy, infrared spectroscopy, gel permeation chromatography, viscosity test, differential scanning calorimetry analysis and thermogravimetric analysis. The results showed that the FEC-PSA resin had good processing performance with processing window of 140 ℃. The viscosity FEC-PSA at 90 ℃ was lower than 50 mPa·s. However, the initial curing temperature was higher than 290 ℃. The curing temperature of FEC-PSA could be obviously decreased with the addition of catalysts. Compared with FEC-PSA thermally cured at high temperature, the initial curing temperature(T_(i))and peak curing temperature(T_(p))of FEC-PSA could be decreased by 70 ℃ and 100 ℃, respectively, when bis(triphenyl phosphine)dicarbonyl nickel was added into the resin. The 5% thermal weight loss temperature(T_(d5)) and 800 ℃ residual rate(Y_(r800℃)) could be increased by 537 ℃ and 87%, respectively. The Tiand Tpof the FEC-PSA could be decreased by more than 70 ℃ by biscyclopentadiene cobalt catalyst. The T_(i) and T_(p) of the cured FEC-PSA could be increased to 495 ℃ and 86%, respectively.
作者
杨唐俊
袁荞龙
黄发荣
YANG Tang-jun;YUAN Qiao-long;HUANG Fa-rong(Key Laboratory of Specially Functional Polymeric Materials and Their Related Technology(Ministry of Education),School of Materials Science and Engineering,East China University of Science and Technology,Shanghai 200237,China)
出处
《热固性树脂》
CAS
CSCD
北大核心
2022年第2期17-23,共7页
Thermosetting Resin
基金
中央高校基本科研业务费专项资金(JKD01211701)。
关键词
含硅芳炔树脂
苯乙炔封端
催化固化
热稳定性
silicon-containing polyarylacetylene
phenylethynyl terminated
catalytic cure reaction
thermal stability
