木质素基含氮磷阻燃剂的合成及热重分析

doi:10.3969/j.issn.0253-2417.2021.03.009

Abstract

Abstract:

Using depolymerized lignin(DL) as raw material, Schiff base nitrogen-containing lignin(N-DL) was prepared by phase transfer ultrasonic method, and then further reacted with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO) to synthesize nitrogen-phosphorus modified DL(NP-DL). NP-DL was a new type of expanded lignin-based nitrogen and phosphorus flame retardant. The structure and performance of NP-DL were characterized by FT-IR, ¹H NMR, ³¹P NMR, TG, TG/FT-IR, TG/MS, GPC and XPS. The results showed that N and P were successfully introduced into the depolymerized lignin; TG analysis showed that the carbon residue rates of NP-DL at 600 and 800℃ were increased by 1 285.5% and 362.6% compared with those of DL, respectively. The test results of TG/FT-IR and TG/MS showed that NP-DL was thermally degraded to produce phosphorus: [OP⁺] with m/z=47, [H₃PO] with m/z=50, [O₂P⁺] with m/z=63 and[HO₂P⁺] with m/z=64 proved that the phosphorus-containing compounds produced during the pyrolysis of NP-DL inhibited combustion.

Key words: lignin, flame retardant, DOPO, Schiff base reaction

CLC Number:

TQ35

Zhuo LI, Shuxian WENG, Fei SONG, Xiaoli REN, Xiaohui YANG, Lihong HU. Synthesis and Thermal Analysis of Lignin-based Flame Retardant Containing Nitrogen and Phosphorus[J]. Chemistry and Industry of Forest Products, 2021, 41(3): 63-70.

Figures/Tables 11

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References 26

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样品 samples	M_n	M_w/M_n	N/%	C/%	H/%	P/%
DL	1748	6.99	1.04	58.37	5.47	—
N-DL	2012	7.56	4.27	57.55	5.96	—
NP-DL	2154	9.29	3.25	58.14	5.59	1.1

样品 samples	T_-5%/℃	T_max/℃			残炭率residual mass/%
样品 samples	T_-5%/℃	StepⅠ	StepⅡ	StepⅢ	600 ℃	800 ℃
DL	199.07	72.6	269.3	471.9	2.28	2.27
N-DL	158.01	78.1	242.3	512.9	10.90	4.19
NP-DL	175.88	70.6	374.8	578.5	31.59	10.50

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Synthesis and Thermal Analysis of Lignin-based Flame Retardant Containing Nitrogen and Phosphorus

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