吡咯亚胺钒络合物催化制备含功能性乙氧基硅烷聚乙烯

刘智颖; 范宏

doi:10.11949/j.issn.0438-1157.20160906

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吡咯亚胺钒络合物催化制备含功能性乙氧基硅烷聚乙烯

材料化学工程与纳米技术 | 更新时间：2025-12-10

- 吡咯亚胺钒络合物催化制备含功能性乙氧基硅烷聚乙烯
- Preparation of functional ethoxysilane-containing polyethylene through ethylene coordination copolymerization catalyzed by iminopyrrolide vanadium complex
- 化工学报 2017年第2期页码：774-780
- 作者机构：
  
  化学工程联合国家重点实验室, 浙江大学化学工程与生物工程学院,浙江,杭州,310027
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20160906
  中图分类号： Q325.1
- 网络首发：2017-02-05，
  
  纸质出版：2017-02-05
- 稿件说明：
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刘智颖, 范宏. 吡咯亚胺钒络合物催化制备含功能性乙氧基硅烷聚乙烯[J]. 化工学报, 2017,(2):774-780.

LIU Zhiying, FAN Hong. Preparation of functional ethoxysilane-containing polyethylene through ethylene coordination copolymerization catalyzed by iminopyrrolide vanadium complex[J]. CIESC Journal, 2017, (2): 774-780.
刘智颖, 范宏. 吡咯亚胺钒络合物催化制备含功能性乙氧基硅烷聚乙烯[J]. 化工学报, 2017,(2):774-780. DOI： 10.11949/j.issn.0438-1157.20160906.

LIU Zhiying, FAN Hong. Preparation of functional ethoxysilane-containing polyethylene through ethylene coordination copolymerization catalyzed by iminopyrrolide vanadium complex[J]. CIESC Journal, 2017, (2): 774-780. DOI： 10.11949/j.issn.0438-1157.20160906.

摘要

通过二甲基乙氧基硅烷与1，7-辛二烯的硅氢加成反应，制备出一种含功能性基团的极性单体——7-辛烯基乙氧基二甲基硅烷（OEMS），在吡咯亚胺钒络合物（VCIP）的催化作用下，该单体可与乙烯配位共聚制备含功能性乙氧基硅烷的乙烯共聚物（PE-co-OEMS）。通过高温核磁共振氢谱及碳谱（1H NMR和13C NMR）、高温凝胶渗透色谱（HT-GPC）和热分析（DSC）等测试方法对共聚物的结构和热性能进行了表征。结果显示，当共单体OEMS的投料量增大至60 mmol·L-1时，共聚反应活性仍可保持在1.2 kg·mmol-1·h-1，OEMS单体插入率为1.3%（摩尔分数）；此外，OEMS投料量对于共聚物的分子量（Mw）和分子量分布（PDI）均具有较大的影响，当OEMS投料量为30 mmol·L-1时，共聚物Mw为16900，PDI为2.1；若继续增大共单体的投料量，共聚物分子量增大且分子量分布变宽。熔点（Tm）和结晶焓（ΔHc）随着OEMS插入率的增大而降低。在三氟甲磺酸作用下，PE-co-OEMS交联后凝胶含量接近100%。

Abstract

A well-defined silane-functionalized comonomer

7-octenylethoxydimethylsilane (OEMS)

was synthesized through hydrosilylation reaction of dimethylethoxysilane with 1

7-octadiene. Catalyzed by a vanadium complex bearing iminopyrrolide ligands (VCIP)

the functional ethoxysilane-containing polyethylenes (PE-co-OEMS) were synthesized by copolymerization of ethylene with OEMS. The structure and properties of PE-co-OEMSs were characterized with 1H NMR

13C NMR

HT-GPC and DSC. It was found that catalytic activity still remained 1.2 kg·mmol-1·h-1 when OEMS feeding reached to 60 mmol·L-1

and the OEMS incorporating in the copolymer was 1.3%(mol). Besides

the OEMS feeding had a great influence on the average molecular weight (Mw) and distribution (PDI) of copolymers. The Mw and PDI of PE-co-OEMS were 16900 and 2.1 when OEMS feeding was 30 mmol·L-1. With further increasing the OEMS feeding

Mw increased and PDI became wider. The melting temperature (Tm) and crystallization enthalpy (ΔHc) decreased with the increase of OEMS incorporation. The ethoxysilane-containing copolymers were easily crosslinked under the catalysis of trifluoromethanesulfonic acid

and the copolymer gel contents after crosslinking were nearly 100%.

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