含二氮杂萘酮联苯结构耐高温、可溶解嵌段聚芳醚酮的合成

鲍锋; 刘程; 宋媛媛; 邬祚强; 王锦艳; 蹇锡高

doi:10.11777/j.issn1000-3304.2017.17265

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含二氮杂萘酮联苯结构耐高温、可溶解嵌段聚芳醚酮的合成

研究论文 | 更新时间：2021-01-26

- 含二氮杂萘酮联苯结构耐高温、可溶解嵌段聚芳醚酮的合成
- Synthesis of Phthalazinone-containing Poly(aryl-ether-ketone) Block Copolymers with Good Solubility and High Thermal Stability
- 高分子学报 2018年0卷第6期页码：692-699
- 作者机构：
- 作者简介：
  
  E-mail: wangjinyan@dlut.edu.cn Jin-yan Wang, E-mail: wangjinyan@dlut.edu.cn
  E-mail: jian4616@dlut.edu.cn Xi-gao Jian, E-mail: jian4616@dlut.edu.cn
- 基金信息：
  
  国家重点基础研究发展计划(863计划，项目号 2015AA033802)、国家重点研发计划(项目号 2017YFB0307600)和科技部重点领域创新团队(项目号 2016RA4053)资助()
- DOI：10.11777/j.issn1000-3304.2017.17265
  中图分类号：
- 纸质出版日期：2018-6，
  
  收稿日期：2017-9-14，
  
  修回日期：2017-10-9，
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鲍锋, 刘程, 宋媛媛, 邬祚强, 王锦艳, 蹇锡高. 含二氮杂萘酮联苯结构耐高温、可溶解嵌段聚芳醚酮的合成[J]. 高分子学报, 2018,0(6):692-699.

Feng Bao, Cheng Liu, Yuan-yuan Song, Zuo-qiang Wu, Jin-yan Wang, Xi-gao Jian. Synthesis of Phthalazinone-containing Poly(aryl-ether-ketone) Block Copolymers with Good Solubility and High Thermal Stability[J]. Acta Polymerica Sinica, 2018,0(6):692-699.
鲍锋, 刘程, 宋媛媛, 邬祚强, 王锦艳, 蹇锡高. 含二氮杂萘酮联苯结构耐高温、可溶解嵌段聚芳醚酮的合成[J]. 高分子学报, 2018,0(6):692-699. DOI： 10.11777/j.issn1000-3304.2017.17265.

Feng Bao, Cheng Liu, Yuan-yuan Song, Zuo-qiang Wu, Jin-yan Wang, Xi-gao Jian. Synthesis of Phthalazinone-containing Poly(aryl-ether-ketone) Block Copolymers with Good Solubility and High Thermal Stability[J]. Acta Polymerica Sinica, 2018,0(6):692-699. DOI： 10.11777/j.issn1000-3304.2017.17265.

摘要

从分子设计的角度出发，设计、合成了3种不同嵌段长度的耐高温、可溶解的嵌段共聚物PPENK-

-PEEKK，成功地将含二氮杂萘酮联苯结构聚芳醚酮PPENK链段与结构规整PEEKK链段进行结合. 首先采用溶液聚合方法合成了羟基封端聚醚醚酮酮(PEEKK-OH)低聚物，并通过正交实验对聚合工艺进行了优化，获得了最优的合成条件. 然后，采用一锅分步加料的方法，合成了PPENK-

-PEEKK嵌段共聚物. 红外测试结果表明了共聚物的成功合成，广角X射线衍射(WXRD)测试结果表明3种共聚物均存在结晶结构. 示差扫描量热仪(DSC)测试结果显示3种共聚物均只有一个玻璃化转变温度(

) (较PEEKK的

有较大的提升)，且存在熔点，具有潜在的热成型加工性能. 热重分析仪(TGA)测试结果表明，3种共聚物的

d5%

、

d10%

分别为491 ~ 510、523 ~ 530 °C，800 °C残炭为63% ~ 65%，共聚物具有优异的热稳定性. 溶解性测试结果显示，共聚物常温即可溶解在

-甲基吡咯烷酮(NMP)中，加热可以促进其溶解，可作为基体树脂用于制备纤维增强复合材料.

Abstract

Through molecular design

three different block copolymers PPENK-

-PEEKK with phthalazinone moiety were synthesized

via

modest polycondensation reaction from the two macromers PEEKK-OH and PPENK-F. Hydroxy terminated PEEKK-OH macromer was obtained by solution polymerization from HQ and BFBB with sulfolane as the solvent. And the molecular weight of PEEKK-OH was successfully controlled by adjusting the monomer ratio

and the polymerized conditions were optimized by orthogonal experiments. While different molecular weight PPENK-F macromer

endcapped with ―F groups

was prepared from DHPZ

DFK and DFBN. Chemical structures and properties of these block copolymers were inverstigated by Fourier transforming infrared spectrum (FTIR)

wide X-ray diffraction (WXRD)

differantial scanning calorimetry (DSC) and thermogravimetric analyses (TGA). The FTIR spectra confirmed the formation of the block copolymers. Furthermore

WXRD measurement showed that all the block copolymers presented crystalline structure

and the crystallinity of the coplolymers decreased with increasing molecular weight of PPENK-F chain segments. All the block copolymers showed only one glass transition temperature (

)

above that of PEEKK-OH. The

of the block copolymers increased with the molecular weight of PPENK-F

due to the introduction of PPENK chain segments into the block copolymers. Moreover

for the reason of of PEEKK incorporation

all these copolymers have a same melting point (

) of about 340 °C

which would facilitate their thermal processing. Besides

all the three copolymers also exhibited remarkable thermal stability in nitrogen atmosphere with the

d5%

weight loss temperature ranging from 491 °C to 510 °C

and

d10%

from 523 °C to 530 °C

respectively. The char yields of the three copolymers at 800 °C were higher than 63%. Finally

all the copolymers showed improved solubility in selectively tested organic solvents

such as NMP and sulfolane

due to the introduction of twisted and non-coplanar DHPZ structure. Consequently

theses materials are potential candidates for the aerospace applications.

关键词

二氮杂萘联苯结构嵌段共聚物聚芳醚耐高温溶解性

Keywords

PhthalazinoneBlock copolymerPoly(aryl ether)Heat-resistantSolubility

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