木质素基膨胀型阻燃剂的制备及其应用

doi:10.3969/j.issn.0253-2417.2021.04.002

林产化学与工业 ›› 2021, Vol. 41 ›› Issue (4): 10-16.doi: 10.3969/j.issn.0253-2417.2021.04.002

木质素基膨胀型阻燃剂的制备及其应用

梁孟珂¹, 陈静¹, 戴鹏¹, 马晓峰¹^,², 张猛³, 罗振扬¹^,²^,*()

1. 南京林业大学理学院, 江苏南京 210037
2. 南京林业大学高分子材料研究所, 江苏南京 210037
3. 中国林业科学研究院林产化学工业研究所, 江苏南京 210042

收稿日期:2020-10-22 出版日期:2021-08-28 发布日期:2021-08-31
通讯作者: 罗振扬 E-mail:luozhenyang@njfu.edu.cn
作者简介:罗振扬, 教授, 硕士生导师, 主要从事生物质高分子材料研究工作; E-mail: luozhenyang@njfu.edu.cn
梁孟珂(1999-), 男, 山西太原人, 本科生, 从事高分子材料与工程专业研究
基金资助:
国家重点研发计划资助项目(2018YFD0600402);南京林业大学大学生实践创新训练计划项目(202010298179H)

Preparation and Application of Lignin-based Intumescent Flame Retardant

Mengke LIANG¹, Jing CHEN¹, Peng DAI¹, Xiaofeng MA¹^,², Meng ZHANG³, Zhenyang LUO¹^,²^,*()

1. College of Science, Nanjing Forestry University, Nanjing 210037, China
2. Institute of Polymer Materials, Nanjing Forestry University, Nanjing 210037, China
3. Institute of Chemical Industry of Forest Products, CAF, Nanjing 210042, China

Received:2020-10-22 Online:2021-08-28 Published:2021-08-31
Contact: Zhenyang LUO E-mail:luozhenyang@njfu.edu.cn

摘要/Abstract

摘要：

以木质素作为膨胀型阻燃剂的基体，通过接枝氮、磷元素成功合成了碳源、酸源、气源三位一体的木质素基膨胀型阻燃剂Lig-T，实现了良好的阻燃性能。通过红外光谱（FT-IR）分析、元素分析和X射线光电子能谱（XPS）分析证明阻燃剂Lig-T的结构。将木质素基膨胀型阻燃剂按照不同质量分数添加到环氧树脂（EP）中制备Lig-T/EP复合材料，以热重（TG）分析、UL-94垂直燃烧测试、氧指数（LOI）测试和锥形量热（Cone）测试考察复合材料的热稳定性能和阻燃性能。研究结果表明：当木质素基膨胀型阻燃剂Lig-T质量分数为20%时Lig-T/EP复合材料（20% Lig-T/EP）便能达到UL-94的V-0级别，且LOI值高达28.5%，残余物质量分数从14.8%提高到20.2%；随着Lig-T质量分数的增加，复合材料在燃烧过程中热释放总量、烟释放总量均呈现下降的趋势。

关键词: 木质素, 曼尼希反应, 膨胀型阻燃剂, 环氧树脂

Abstract:

Lignin-based intumescent flame retardant(Lig-T) with carbon source, acid source and gas source was synthesized successfully by grafting nitrogen and phosphorus elements. The structure of the flame retardant Lig-T was proved by Fourier transform infrared spectrometer(FT-IR), elements analysis and X-ray photoelectron spectroscopy(XPS). The Lig-T was added to the epoxy resin with different mass fractions to obtain Lig-T/EP composite material. Thermogravimetric analysis, underwriters laboratories 94(UL-94) vertical buring test, oxygen index(LOI) test and cone calorimetry(Cone) test were used to investigate the thermal stability and flame retardancy of composite materials. The results showed that when the mass fraction of the Lig-T was 20%, the composite material 20% Lig-T/EP could reach the UL-94 V-0 level, the oxygen index value was as high as 28.5%, and the mass fraction of the residue increased from 14.8% to 20.2%.With the increase of the mass fraction of Lig-T, the total amount of heat release and the total amount of smoke released during the combustion process of the composite material decreased.

Key words: lignin, Mannich reaction, intumescent flame retardant, epoxy resin

中图分类号:

TQ35
TQ314.1

梁孟珂, 陈静, 戴鹏, 马晓峰, 张猛, 罗振扬. 木质素基膨胀型阻燃剂的制备及其应用[J]. 林产化学与工业, 2021, 41(4): 10-16.

Mengke LIANG, Jing CHEN, Peng DAI, Xiaofeng MA, Meng ZHANG, Zhenyang LUO. Preparation and Application of Lignin-based Intumescent Flame Retardant[J]. Chemistry and Industry of Forest Products, 2021, 41(4): 10-16.

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样品sample	C/%	H/%	N/%
Lig-F	64.20	5.98	1.46
Lig-S	72.48	5.76	5.14
Lig-T	62.44	5.45	3.53

样品 samples	T_i/℃	T_max/℃	残留物(800 ℃)/% residue
EP	384	389	14.8
5% Lig-T/EP	375	386	15.5
10% Lig-T/EP	371	382	19.0
15% Lig-T/EP	365	373	19.1
20% Lig-T/EP	355	365	20.2

样品 samples	UL-94				LOI/%
样品 samples	级别rating	t1/s	t2/s	熔滴droplet	LOI/%
EP	无级别no rating	130	34	是yes	22.3
5% Lig-T/EP	无级别no rating	100	22	是yes	23.8
10% Lig-T/EP	V-1	30	21	否no	24.2
15% Lig-T/EP	V-1	25	18	否no	26.5
20% Lig-T/EP	V-0	10	9	否no	28.5

样品 samples	初始峰值热释放速率/(kW·m^-2) initial peak heat release rate	平均热释放速率/(kW·m^-2) average heat release rate	热释放总量/(MJ·m^-2) total heat release	峰值烟释放速率/(m²·s^-1) peak of smoke production rate	烟释放总量/m² total smoke rate
EP	1959.75	325.64	60.80	0.513	2503.16
5% Lig-T/EP	1846.32	295.87	46.99	0.470	1897.77
10% Lig-T/EP	1810.26	245.40	44.59	0.406	1715.68
15% Lig-T/EP	1545.82	184.24	43.14	0.403	1712.40
20% Lig-T/EP	1373.83	176.18	41.63	0.354	1633.64

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木质素基膨胀型阻燃剂的制备及其应用

Preparation and Application of Lignin-based Intumescent Flame Retardant

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