Effect of AlPO⁃based zeolites on flame⁃retardancy and thermal stability of polypropylene composites

doi:10.19491/j.issn.1001-9278.2022.12.010

Abstract

Abstract:

AlPO⁃based zeolites （AlPO⁃n， n=5， 11， 17， and 34） were prepared through hydrothermal synthesis. The obtained products were incorporated into polypropylene （PP） to prepare the intumescent flame⁃retardant composites for enhancing its flame retardancy and thermal stability. The flammability and mechanical properties of the composites were evaluated through limiting oxygen index， vertical burning test， cone calorimetry， and tensile test. The results indicated that the PP composite containing 1 wt % AlPO⁃17 achieved a significantly enhancement in LOI and char residue， which increased by 34.8 % and 14.3 %， respectively， compared to pure PP.

Key words: AlPO?based zeolites, polypropylene, flame retardancy, thermal stability

CLC Number:

TQ 325.1⁺4

GONG Shaofeng, TENG Xia, TANG Wufei. Effect of AlPO⁃based zeolites on flame⁃retardancy and thermal stability of polypropylene composites[J]. China Plastics, 2022, 36(12): 65-70.

Figures/Tables 15

样品	磷源	铝源	模板剂	晶化温度/℃	晶化时间/h
AlPO⁃5	磷酸	异丙醇铝	三乙胺	180	24
AlPO⁃11	磷酸	异丙醇铝	二正丙胺	180	48
AlPO⁃17	磷酸	异丙醇铝	环己胺	200	96
AlPO⁃34	磷酸	氢氧化铝	吗啉	195	120

Tab.1. Synthesis materials and crystallization conditions of AlPO⁃n

样品	n_Al/mol	n_P/mol	n_R/mol	n $H 2 O$ /mol
AlPO⁃5	2	2	2.0	50
AlPO⁃11	2	2	1.0	50
AlPO⁃17	2	2	1.0	60
AlPO⁃34	1	1	1.25	50

样品	n_Al/mol	n_P/mol	n_R/mol	n $H 2 O$ /mol
AlPO⁃5	2	2	2.0	50
AlPO⁃11	2	2	1.0	50
AlPO⁃17	2	2	1.0	60
AlPO⁃34	1	1	1.25	50

Tab.2. The ratio of preparation for AlPO⁃n

样品编号	PP/%	IFR/%	AlPO⁃5/ %	AlPO⁃11/%	AlPO⁃17/%	AlPO⁃34/%
1^#	100	0	0	0	0	0
2^#	75	25（APP∶PER=2∶1）	0	0	0	0
3^#	75	25（APP∶PER=3∶1）	0	0	0	0
4^#	75	25（APP∶PER=4∶1）	0	0	0	0
5^#	75	24（APP∶PER=3∶1）	1	0	0	0
6^#	75	24（APP∶PER=3∶1）	0	1	0	0
7^#	75	24（APP∶PER=3∶1）	0	0	1	0
8^#	75	24（APP∶PER=3∶1）	0	0	0	1

Tab.3. The formulation of PP/IFR composites containing AlPO⁃n

Fig.1. XRD patterns of AlPO⁃n with different pore size

Fig.2. FTIR of AlPO⁃n with different pore size

AlPO⁃n类型	AlPO⁃5	AlPO⁃11	AlPO⁃17	AlPO⁃34
S_BET/m²·g^-1	274	210	642	341

Tab.4. SBET value of AlPO⁃n

样品	PP/%	IFR/%	AlPO⁃5/%	AlPO⁃11/%	AlPO⁃17/%	AlPO⁃34/%	LOI/%	UL 94
1^#	100	0	0	0	0	0	17.9±0.2	NR
2^#	75	25（APP∶PER=2∶1）	0	0	0	0	29.5±0.2	V⁃2
3^#	75	25（APP∶PER=3∶1）	0	0	0	0	30.8±0.2	V⁃2
4^#	75	25（APP∶PER=4∶1）	0	0	0	0	28.8±0.2	V⁃2
5^#	75	24（APP∶PER=3∶1）	1	0	0	0	32.6±0.2	V⁃0
6^#	75	24（APP∶PER=3∶1）	0	1	0	0	33.1±0.2	V⁃0
7^#	75	24（APP∶PER=3∶1）	0	0	1	0	34.2±0.2	V⁃0
8^#	75	24（APP∶PER=3∶1）	0	0	0	1	33.4±0.2	V⁃0

Tab.5. LOI and UL 94 tests of PP composites

Fig.3. HRR results of PP and its composites

Fig.4. FTIR of char residues of PP/IFR/AlPO⁃n composites after LOI tests

Fig.5. Photos of char residues of PP/IFR/AlPO⁃n composites after LOI tests

Fig.6. Photos of PP， PP/IFR and PP/IFR/ AlPO⁃17 systems before and after being heated at different temperature

Fig.7. FTIR spectra of condensed phases of PP/IFR and PP/IFR/AlPO⁃17 systems obtained after being heated at different temperature

Fig.8. TGA curves of PP and its composites （in N2）

样品	T_5%	T_10%	T_50%	600 ℃残炭率（W_600℃）/%
PP	380	400	420	0
PP/IFR	290	360	440	6.8
PP/IFR/AlPO⁃17	330	390	450	14.3

Tab.6. TGA main data of PP and its composites

样品	拉伸强度/MPa	断裂伸长率/%
PP	35.2	19.1
PP/IFR （75/25）	23.5	14.3
PP/IFR/AlPO⁃17 （75/24/1）	25.1	15.2

Tab.7. Tensile strength and elongation at break of PP and its composites

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