Synthesis of Micro- to Nano-scale Perovskite Calcium Hydroxytinate and Its Performance as a Flame Retardant in Epoxy Resin

doi:10.7503/cjcu20200470

Abstract

Abstract:

Perovskite hydroxystannate is a new type of flame retardant and smoke suppressant with high efficiency that has appeared in recent years. In this paper， micro- to nano-scale perovskite-type calcium hydroxystannate［CaSn（OH）₆， CSH］ was synthesized by co-precipitation method. Scanning electron micros-copy， transmission electron microscopy， X-ray diffraction， infrared spectroscopy， and X-ray photoelectron spectroscopy were used to characterize its morphology and structure. The results show that the synthesized CaSn（OH）₆ was a pure regular hexahedron with an average particle size of 500 nm， and showed a uniform size and good dispersion. CSH/EP flame retardant composites were prepared by applying CaSn（OH）₆ to epoxy resin（EP）. Thermogravimetric analysis， limiting oxygen index and cone calorimeter tests were used to characte-rized its thermal degradation behavior and combustion performance， respectively， scanning electron micros-copy， infrared spectroscopy， X-ray diffraction and Raman spectroscopy were used to explore the carbonizing flame retardant mechanism of EP composites. The results show that CaSn（OH）₆ could significantly improve the high temperature stability， heat release rate， total heat release， total smoke release and limiting oxygen index value of the EP composites. Especially at very low addition levels（0.5%， mass fraction）， the flame retardant and smoke suppression performance were greatly improved， and the heat release rate， total heat release and carbon monoxide release were reduced by 45.8%， 25.1% and 31.3%， respectively. Moreover， due to the good dispersion of CaSn（OH）₆ in the EP matrix and the strong interface effect， the addition of CaSn（OH）₆ also improved the mechanical strength of the EP composite and enhanced its flame retarancy properties. The CaSn（OH）₆ synthesized in this paper can be used as a multi-functional high-efficiency flame retardant， smoke suppression as well as a reinforcing agent for EP resin.

Key words: Epoxy resin, Calcium hydroxystannate, Flame retardant, Perovskite （Ed.： W, K, M）

CLC Number:

O631.2

TrendMD:

DONG Luming, SU Yanyue, WANG Chunzheng, QIAO Yafei, CHEN Yajun, MA Haiyun. Synthesis of Micro- to Nano-scale Perovskite Calcium Hydroxytinate and Its Performance as a Flame Retardant in Epoxy Resin[J]. Chem. J. Chinese Universities, 2021, 42(3): 937.

Figures/Tables 11

References 28

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Sample	T_5%/℃	T_max/℃	Char yield(%)
CaSn(OH)₆	233.1	290.0	73.6
Pure EP	362.1	371.8	10.9
0.5%CSH/EP	358.8	371.9	11.3
1%CSH/EP	359.5	372.7	12.3
3%CSH/EP	357.8	375.8	13.5
5%CSH/EP	358.2	377.0	14.2

Sample	T_5%/℃	T_max/℃	Char yield(%)
CaSn(OH)₆	233.1	290.0	73.6
Pure EP	362.1	371.8	10.9
0.5%CSH/EP	358.8	371.9	11.3
1%CSH/EP	359.5	372.7	12.3
3%CSH/EP	357.8	375.8	13.5
5%CSH/EP	358.2	377.0	14.2

Sample	PHRR/(kW·m^-2)	THR/(MJ·m^-2)	SPR/(m²·s^-1)	TSP/m²	COP/(g·s^-1)	Mass loss, w(%)
EP	1423.40	124.35	0.35	33.28	0.032	8.5%
0.5%CSH/EP	771.02	93.19	0.32	29.43	0.022	12.7%
1%CSH/EP	659.54	89.20	0.29	28.65	0.019	16.3%
5%CSH/EP	589.64	79.47	0.26	27.33	0.015	23.9%

Sample	PHRR/(kW·m^-2)	THR/(MJ·m^-2)	SPR/(m²·s^-1)	TSP/m²	COP/(g·s^-1)	Mass loss, w(%)
EP	1423.40	124.35	0.35	33.28	0.032	8.5%
0.5%CSH/EP	771.02	93.19	0.32	29.43	0.022	12.7%
1%CSH/EP	659.54	89.20	0.29	28.65	0.019	16.3%
5%CSH/EP	589.64	79.47	0.26	27.33	0.015	23.9%

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