Synthesis of Porous and Siloxane-containing Polyurea through Precipitation Polymerization

Xin Qi; Li-li Wu; Shu-sheng Li; Xiang-zheng Kong

doi:10.11777/j.issn1000-3304.2018.18271

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Synthesis of Porous and Siloxane-containing Polyurea through Precipitation Polymerization

Research Article | 更新时间：2021-01-26

- Synthesis of Porous and Siloxane-containing Polyurea through Precipitation Polymerization
- Acta Polymerica Sinica Vol. 50, Issue 7, Pages: 730-739(2019)
- 作者机构：
  
  1.济南大学化学化工学院　济南 250022
  2.山东省产品质量检验研究院　济南 250102
- 作者简介：
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2018.18271
  CLC：
- Published：2019-7，
  
  Published Online：21 January 2019，
  
  Received：18 December 2018，
  
  Revised：21 December 2018，
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Xin Qi, Li-li Wu, Shu-sheng Li, Xiang-zheng Kong. Synthesis of Porous and Siloxane-containing Polyurea through Precipitation Polymerization. [J]. Acta Polymerica Sinica 50(7):730-739(2019)
DOI：

Xin Qi, Li-li Wu, Shu-sheng Li, Xiang-zheng Kong. Synthesis of Porous and Siloxane-containing Polyurea through Precipitation Polymerization. [J]. Acta Polymerica Sinica 50(7):730-739(2019) DOI： 10.11777/j.issn1000-3304.2018.18271.

摘要

通过甲苯二异氰酸酯(TDI)与

-氨丙基二硅氧烷(APDS)在水-丙酮混合溶剂中沉淀聚合制备了含有机硅聚脲多孔材料(PUS). 研究了两单体质量比和混合溶剂中水/丙酮质量比及反应温度对PUS产率及形貌的影响. 使用扫描电镜和红外光谱及核磁共振对PUS的形貌及化学结构进行了表征. 结果表明，在反应温度30 °C和水/丙酮质量比为3/7条件下，改变APDS/TDI的质量比，可控制PUS的形貌. 当APDS/TDI配比小于3/7时可制得为无规则形状的多孔结构PUS；而APDS/TDI高于3/7时可制得PUS多孔微球；APDS/TDI配比为4/6时多孔微球粒径分布最为均一，其比表面为106 m

/g. 此外，微球粒径随着水/丙酮配比及反应温度的升高而逐渐减小. 对PUS热性能表征结果表明其具有良好的耐热性.

Abstract

Poly(urea-siloxane) (PUS) was prepared through the precipitation polymerization between

-aminopropyl disiloxane (APDS) and toluene diisocyanate (TDI) in H

O-acetone mixed solvent

which involved no extra addition of surfactants

initiators

or any other additives. Effects of monomer ratio (APDS/TDI

)

binary solvent composition ratio (H

O/acetone

)

and reaction temperature on the polymerization process and PUS morphology were investigated. Results indicated that tuning the APDS/TDI ratio could readily change the PUS morphology from a porous irregular form into porous microspheres. Specifically

the former appeared at APDS/TDI weight ratio no more than 2/8

while the latter occurred when increasing the APDS/TDI ratio up to 3/7 or higher; APDS/TDI ratio at 4/6 could affard porous PUS microspheres with 1 µm in diameter and narrow polydispersity. On the other hand

O/acetone weight ratio and polymerization temperature also affected the size and size distribution of PUS microspheres remarkably

and the the narrowest size distribution of 1.04 was realized at APDS/TDI ratio of 4/6

O/acetone ratio of 3/7

and polymerization temperature equal to 30 °C. With APDS/TDI ratio varied from 0/10 to 4/6

the pore volume of PUS increased from about 1.79 cm

/g to 2.36 cm

whereas the specific surface area decreased from about 163.00 m

/g to 106.18 m

/g. On the basis of polymerization process

the changes in PUS morphology and porous properties versus APDS/TDI ratio variation could be well interpreted through the mechanisms of polymer precipitation and pore formation. PUS chemical structure was revealed by FTIR and NMR

while thermal property characterization indicated an enhanced thermal stability with the incorporation of APDS units into polyurea system.

关键词

沉淀聚合聚脲有机硅聚合物微球多孔结构

Keywords

Precipitation polymerizationPolyureaSiloxanePolymer microspheresPorous structure

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Related Institution

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