对位芳纶气凝胶粉体的制备与性能研究

doi:10.11949/0438-1157.20211071

摘要/Abstract

摘要：

以对位芳纶纳米纤维(PANF)水凝胶为原料，将冻凝胶粉碎法与冷冻干燥法相结合，制备出PANF气凝胶粉体。系统研究了对位芳纶气凝胶粉体的微观结构及性能参数，以及制备条件对产物形貌的影响，并初步探究了其应用。结果表明，液氮冷冻制备的PANF气凝胶粉体具有多孔结构，松装密度约为17.0 kg?m^-3，孔隙率约为98.8%，BET比表面积可达126.30 m²?g^-1。PANF气凝胶粉体的耐热性优异，在氮气气氛下500℃前几乎无分解；热导率较低，约为0.03 W?m^-1·K^-1。气凝胶粉体具有吸附罗丹明B等染料的特征，同时可作为纳米填充材料增强聚氨酯乳胶膜等聚合物材料的硬度，其低热导率表明其有望应用于绝热领域。

关键词: 对位芳纶纳米纤维, 气凝胶粉体, 制备, 吸附, 复合材料

Abstract:

Using para-aramid nanofiber (PANF) hydrogel as raw material, the cryogel crushing method and freeze-drying method are combined together to prepare PANF aerogel powder. The microstructure and performance parameters of para-aramid aerogel powder and the influence of preparation conditions on the morphology of the product were systematically studied, and its application was preliminarily explored. The results showed that the aerogel powders have a porous structure. The apparent density, porosity, and Brunauer-Emmett-Teller surface aerogel area are about 17.0 kg?m^-3, 98.8% and 126.30 m²?g^-1, respectively. The thermal stability of aerogel powders is excellent and almost no decomposition occurs before 500°C under nitrogen atmosphere. The thermal conductivity of aerogel powder is as low as 0.03 W?m^-1·K^-1. The aerogel powders can be utilized for the adsorption of some kinds of dyes, such as Rhodamine B. Furthermore, the aerogel powders can be used as nanofiller to improve the mechanical performance of some kinds of polymers, such as the hardness of polyurethane latex film. The low thermal conductivity indicated that the aerogel powder might be applied in the area of thermal insulation.

Key words: para-aramid nanofiber, aerogel powders, preparation, adsorption, composites

中图分类号:

TQ 342⁺.72

谢春杰, 何然, 庹新林, 杨万泰. 对位芳纶气凝胶粉体的制备与性能研究[J]. 化工学报, 2021, 72(12): 6361-6370.

Chunjie XIE, Ran HE, Xinlin TUO, Wantai YANG. Preparation and performance of para-aramid aerogel powders[J]. CIESC Journal, 2021, 72(12): 6361-6370.

图/表 10

图1 PANF气凝胶粉体制备流程图

Fig.1 Preparation process of the PANF aerogel powders

图2 PANF的TEM图（内插图为PANF分散液的照片）

Fig.2 TEM image of the PANF（ The inset is the photograph of the PANF dispersion）

图3 PANF气凝胶粉体的SEM图

Fig.3 SEM images of the PANF aerogel powders

图4 制备工艺对产物的影响

Fig.4 The effect of preparation technology on the product

表1 PANF气凝胶粉体和气凝胶块体的比表面积和孔体积对比

Table 1 Comparison of the surface area and pore volume of PANF aerogel powders and aerogel monoblock

项目	PANF气凝胶粉体	PANF气凝胶块体
BET比表面积 /(m²?g^-1)	126.30	78.92
总孔体积 /(cm³?g^-1)	7.00 ×10^-1①	3.96 ×10^-1②
BJH法累积吸附孔体积 /(cm³?g^-1)	7.03 ×10^-1	4.01 ×10^-1
BJH法累积脱附孔体积 /(cm³?g^-1)	7.08 ×10^-1	4.04 ×10^-1
SF法孔体积 /(cm³?g^-1)	4.15 ×10^-2	2.48 ×10^-2

图5 PANF气凝胶粉体介孔和大孔孔体积分布（内插图为微孔孔体积分布）

Fig.5 Pore volume distribution of mesopores and macropores of PANF aerogel powders（The inset is the pore volume distribution of micropores）

图6 PANF气凝胶粉体和Kevlar纤维的XRD和FTIR谱图

Fig.6 XRD and FTIR spectra of PANF aerogel powders and Kevlar fiber

图7 PANF气凝胶粉体和Kevlar纤维的TGA和DSC曲线

Fig.7 TGA and DSC curves of PANF aerogel powders and Kevlar fiber

图8 罗丹明B染料在PANF气凝胶粉体吸附前后的吸光度变化

Fig.8 Variation of the absorbance of Rhodamine B dye before and after absorbed by PANF aerogel powders

图9 通过纳米压痕法测试的PU乳胶膜和PU/PANF复合乳胶膜的硬度和模量对比

Fig.9 Comparison of the hardness and modulus of the PU latex film and PU/PANF composite latex film tested by nano indentation method

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