Inflame-retardant Water-borne Epoxy Resin of APP Microsphere with Carrageenan Cladding†

doi:10.7503/cjcu20180416

Abstract

Abstract:

After k-carrageenan was purified by barium chloride and degraded by hydrogen oxidation, a series of k-carrageenan/ammonium polyphosphate(k-CM/APP) inflame-retardant microsphere was prepared using inverse emulsion polymerization method. Then k-CM/APP was added to water-borne epoxy resin to prepare EP2, EP3, EP4 steel structure fire retardant coating. The structure and morphology of k-CM/APP were represented by using infrared spectrograph(IR), scanning electron microscope(SEM), energy dispersive spectrometry(EDS). The limit oxygen index(LOI), vertical combustion(UL-94), back temperature test method, thermogravimetry(TG), cone calorimeter, adhesion tester, IR and SEM were used for analyzing the flame retardant property, heat-insulating property, thermal property and mechanical property. Research results showed that k-CM/APP spherical structure was complete, and the carbon residue at 800 ℃ reached 59.5%. Compared with other fire retardant coatings, the LOI of the EP3 fire retardant coating with added k-CM/APP(3/1) reached 28.5%, UL-94 reached the class V-0, and the fire-resistant temperature of 60 min fire retardant coating was 253 ℃. Compared with pure EP coating, the heat release rate peak of EP2 coating was decreased by 58.26% and the total heat release quantity was decreased by 20.84%, adhesion reached 8.74 MPa.

Key words: Carrageenan microsphere, Ammonium polyphosphate, Waterborne epoxy resin, Flame retardancy

CLC Number:

O636

TrendMD:

WANG Na,YANG Fei,ZHANG Jing,FANG Qinghong. Inflame-retardant Water-borne Epoxy Resin of APP Microsphere with Carrageenan Cladding^†[J]. Chem. J. Chinese Universities, 2019, 40(2): 385.

Figures/Tables 11

Scheme 1 Synthesis mechanism of k-CM/APP

Table 1 Formulation of steel fireproof coating*

Sample	m(EP)/g	m(Curing agent)/g	m(H₂O)/g	m(APP)/g	m[k-CM/ APP(2/1)]/g	m[k-CM/ APP(3/1)]/g	m[k-CM/ APP(4/1)]/g
EP0	60	20	20	-	-	-	-
EP1	45	15	20	20	-	-	-
EP2	45	15	20	-	20	-	-
EP3	45	15	20	-	-	20	-
EP4	45	15	20	-	-	-	20

Fig.1 SEM images of k-CM(A), k-CM/APP(2/1)(B), k-CM/APP(3/1)(C) and k-CM/APP(4/1)(D)

Table 2 Elemental analysis data of k-CM, k-CM/APP(2/1), k-CM/APP(3/1) and k-CM/APP(4/1)

Sample	Mass fraction(%)
Sample	S	Ba	P
k-CM	3.94	13.98	0
k-CM/APP(2/1)	3.54	11.18	8.72
k-CM/APP(3/1)	3.48	12.79	7.33
k-CM/APP(4/1)	3.21	12.56	6.36

Table 3 TG data of APP, k-CM/APP(2/1), k-CM/APP(3/1) and k-CM/APP(4/1)*

Sample	Temperature(5%)/℃	Temperature(20%)/℃	w₈₀₀(%)
APP	152.3	282.1	33.5
k-CM/APP(2/1)	170.1	218.8	53.7
k-CM/APP(3/1)	183.9	232.6	59.5
k-CM/APP(4/1)	176.7	228.5	55.7

Table 4 LOI and UL-94 test results of different samples

Sample	LOI(%)	UL-94	Droplet	Sample	LOI(%)	UL-94	Droplet
EP0	19.7	No rating	Yes	EP3	28.5	V-0	No
EP1	30.1	V-0	No	EP4	27.2	V-0	No
EP2	25.9	V-0	No

Scheme 2 Flame retardancy mechanism

Fig.2 Back temperature test of steel(a), EP0(b), EP1(c), EP2(d), EP3(e) and EP4(f)

Fig.3 Cone calorimeter curves of EP0(a), EP1(b) and EP3(c)(A) HRR vs. time; (B) THR vs. time; (C) SPR vs. time; (D) TSR vs. time.

Fig.4 SEM images of surface(A—C) and inside(D—F) of EP0(A, D), EP1(B, E) and EP3(C, F)

Fig.5 SEM images of chars of EP0(A), EP1(B) and EP3(C)

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