Synthesis and characterization of aminopropyl oligomeric silsesquioxane and its amidation products

doi:10.19491/j.issn.1001-9278.2022.08.001

Abstract

Abstract:

Caged aminopropylsilsesquioxane （NH₂-propyl-POSS） was synthesized through one-pot hydrolysis-condensation under alkali-catalyzed conditions using 3-aminopropyltrimethoxysilane as a raw material. The obtained products were characterized using infrared spectroscopy， nuclear magnetic resonance， and electrospray ionization-time of flight mass spectrometry. The results indicated that the synthesized NH₂-propyl-POSS was a cage-structured mixture with different sizes， and the contents of cage structured T8， T9 and T10 were relatively high. Acetylpropyl POSS and propynoyl POSS were further synthesized through the amidation of NH₂-propyl-POSS with acetic acid and propiolic acid， respectively， and their structures were characterized using infrared spectroscopy， ¹H-NMR spectroscopy， and ¹³C-NMR spectroscopy. X-ray diffraction analysis indicated that the three POSSs were all amorphous structures. According to the thermal decomposition characteristics obtained from thermogravimetric analysis， NH₂-propyl-POSS showed the highest thermal stability among the three POSSs. NH₂-propyl-POSS was used for epoxy resin （EP） to improve its thermal stability. The EP/NH₂-propyl-POSS blends exhibited a glass transition temperature of 180.7 oC and a limiting oxygen index of 25.2 vol% with the addition of 5 wt% POSS.

Key words: aminosilsesquioxane, cage structure, thermal property, amidation

CLC Number:

TQ322.4

DONG Youbang, ZHANG Zeqi, YANG Rongjie. Synthesis and characterization of aminopropyl oligomeric silsesquioxane and its amidation products[J]. China Plastics, 2022, 36(8): 1-9.

Figures/Tables 18

References 25

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样品	E⁃44/g	DDS/g	NH₂⁃propyl⁃POSS/g
EP	100	30	0
EP/1 % NH₂⁃propyl⁃POSS	100	30	1.313
EP/3 % NH₂⁃propyl⁃POSS	100	30	4.022
EP/5 % NH₂⁃propyl⁃POSS	100	30	6.842

样品	E⁃44/g	DDS/g	NH₂⁃propyl⁃POSS/g
EP	100	30	0
EP/1 % NH₂⁃propyl⁃POSS	100	30	1.313
EP/3 % NH₂⁃propyl⁃POSS	100	30	4.022
EP/5 % NH₂⁃propyl⁃POSS	100	30	6.842

溶剂	溶解性	溶剂	溶解性
二氯甲烷	-	甲醇	+
丙酮	+	乙醇	+
四氢呋喃	-	水	+
甲苯	-	二甲基亚砜	+

溶剂	溶解性	溶剂	溶解性
二氯甲烷	-	甲醇	+
丙酮	+	乙醇	+
四氢呋喃	-	水	+
甲苯	-	二甲基亚砜	+

m/z值	分子量	类型
763.2	797	T7
863.2	898	T8
881.3	880	T8
1 000.3	999	T9
1 101.3	1 100	T10