Anionic Synthesis of Heptaisobutyl Polyhedral Oligomeric Silsesquioxane Functionalized Polystyrene

Ming-yi Liao; He Zhang

doi:10.11777/j.issn1000-3304.2016.15298

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Anionic Synthesis of Heptaisobutyl Polyhedral Oligomeric Silsesquioxane Functionalized Polystyrene

Research Article | 更新时间：2021-03-19

- Anionic Synthesis of Heptaisobutyl Polyhedral Oligomeric Silsesquioxane Functionalized Polystyrene
- Acta Polymerica Sinica Issue 6, Pages: 722-727(2016)
- 作者机构：
  
  大连海事大学交通运输装备与海洋工程学院大连 116026
- 作者简介：
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2016.15298
  CLC：
- Published：2016-6，
  
  Received：3 November 2015，
  
  Revised：24 December 2015，
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Ming-yi Liao, He Zhang. Anionic Synthesis of Heptaisobutyl Polyhedral Oligomeric Silsesquioxane Functionalized Polystyrene. [J]. Acta Polymerica Sinica (6):722-727(2016)
DOI：

Ming-yi Liao, He Zhang. Anionic Synthesis of Heptaisobutyl Polyhedral Oligomeric Silsesquioxane Functionalized Polystyrene. [J]. Acta Polymerica Sinica (6):722-727(2016) DOI： 10.11777/j.issn1000-3304.2016.15298.

摘要

以苯乙烯为单体、氯丙基七异丁基多面体低聚倍半硅氧烷(chloropropyllsobutyl POSS

POSS-Cl)为封端剂、正丁基锂(

-BuLi)为引发剂、环己烷为溶剂、四氢呋喃(THF)为结构调节剂

采用阴离子聚合技术

合成了POSS端基官能化聚苯乙烯(PS-POSS).采用核磁共振仪(

H-NMR、

C-NMR)和凝胶渗透色谱仪(GPC)对PS-POSS的结构和分子量分布进行了表征

证明了POSS与聚苯环乙烯锂(PSLi)发生了封端反应生成PS-POSS;封端后分子量分布略有加宽

特别是相比传统有机封端剂

没有二聚等副产物生成.考察了引发剂种类、结构调节剂用量、POSS用量、PS分子量、封端反应温度和时间等因素对PS-POSS封端效率的影响.结果表明

在THF/

-BuLi摩尔比大于5、POSS/

-BuLi摩尔比等于1.1、反应温度为60℃、反应时间为30 min时

封端效率最高

达到80%以上;而随着PS数均分子量增加

封端效率逐渐降低.

Abstract

Heptaisobutyl polyhedral oligomeric silsesquioxane functionalized polystyrene (PS-POSS) was prepared by using styrene (PS) as monomers

POSS as terminator

-BuLi as initiator

cyclohexane as solvent and tetrahydrofuran (THF) as structure modifier

via

anionic living polymerization. The PS-POSS was characterized by

H-NMR

C-NMR and GPC. The results of

H-NMR and

C-NMR clearly prove that the reaction of poly(styryl)lithium with Cl-POSS has been carried out and GPC chromatograms show that POSS incorporation into end of PS increased the molecular weight distribution of the PS-POSS. It is noteworthy that no obvious dimeric side-products are observed compared to conventional organic terminator. Then the effects of the species of initiator

the content of structure modifier

the molar ratio of POSS and Li

PS molecular weight

terminating reactive temperature and terminating reactive time on the functionalization efficiency were investigated. The results show that the functionalization efficiency reached the highest point when the molar ratio of THF and

-BuLi was more than 5

the molar ratio of terminator POSS and

-BuLi reached 1.1

the terminating temperature reached 60℃ and the terminating time reached 30 min. It is indicated that the reaction of poly(styryl)lithium with Cl-POSS was over when the terminating time reached 30 min. The highest functionalization efficiency is more than 80 percent. Finally

the functionalization efficiency decreased with DS molecular weight increasing as the other conditions kept unchanged.

关键词

POSSPS负离子聚合端基官能化封端效率

Keywords

POSSPSAnion polymerizationEnd-functionalizationFunctionalization efficiency

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College of Chemistry, Chemical Engineering and Materials Science, State and Local Joint Engineering Laboratory for Novel Functional Polymeric Materials, Suzhou Key Laboratory of Macromolecular Design and Precision Synthesis, Jiangsu Key Laboratory of Advanced Functional Polymer Design and Application, Soochow University

Key Laboratory of Space Applied Physics and Chemistry, Ministry of Education, Key Laboratory of Polymer Science and Technology, Shaanxi Province, Northwestern Polytechnical University

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