纳米三聚氰胺氰尿酸盐的合成、表征及其在酚醛泡沫中的应用<sup>*</sup>

doi:10.11901/1005.3093.2013.857

材料研究学报

2014, Vol. 28

Issue (6): 401-406 DOI: 10.11901/1005.3093.2013.857

本期目录 | 过刊浏览

纳米三聚氰胺氰尿酸盐的合成、表征及其在酚醛泡沫中的应用^*

王正洲^1,²(

),徐少洪²,胡立飞²

1. 同济大学先进土木工程教育部重点实验室上海 200092
2. 同济大学材料科学与工程学院上海 200092

Preparation and Characterization of Nano Melamine Cyanurate and Its Application in Phenolic Foam

Zhengzhou WANG^1,^2,^**(

),Shaohong XU²,Lifei HU²

1. Key Laboratory Advanced Civil Engineering Materials, Ministry of Education, Tongji University, Shanghai 200092
2. School of Materials Science and Engineering, Tongji University, Shanghai 200092

引用本文:

王正洲,徐少洪,胡立飞. 纳米三聚氰胺氰尿酸盐的合成、表征及其在酚醛泡沫中的应用^*[J]. 材料研究学报, 2014, 28(6): 401-406.
Zhengzhou WANG, Shaohong XU, Lifei HU. Preparation and Characterization of Nano Melamine Cyanurate and Its Application in Phenolic Foam[J]. Chinese Journal of Materials Research, 2014, 28(6): 401-406.

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摘要:

以三聚氰胺和氰尿酸为原料, 采用溶剂热方法制备出纳米三聚氰胺氰尿酸盐(NMC)。分别利用傅里叶变换红外光谱(FTIR)、X射线衍射(XRD)、扫描电镜(SEM)等手段对其组成和结构进行表征, 研究了不同溶剂(蒸馏水、无水乙醇和苯)、不同类型的表面活性剂(十二烷基硫酸钠(SDS)、十六烷基三甲基溴化铵(CTAB)、壬基酚聚氧乙烯醚(NP))、反应温度和反应时间对产物粒径的影响。结果表明, 只有用水为溶剂才能合成出NMC; 采用苯和无水乙醇溶剂时产物的粒径较大, 为微米级。用CTAB和SDS为表面活性剂制备的产物平均粒径约为100 nm, 而用NP活性剂制备的产物平均粒径则达到3.1 μm。制备NMC合适的反应温度为150℃, 反应时间为1-3 h。比较了NMC和微米级三聚氰胺氰尿酸盐(MMC)在增韧酚醛泡沫中的阻燃性能和力学性能。结果表明, 与MMC增韧酚醛泡沫相比, NMC阻燃增韧酚醛泡沫的氧指数和弯曲强度都有所提高。

关键词 ：有机高分子材料, 材料合成, 纳米三聚氰胺氰尿酸盐, 溶剂热方法, 酚醛泡沫

Abstract：

Nano melamine cyanurate (NMC) was synthesized by a solvothermal method, and characterized by FTIR, XRD and SEM. The effect of solvents, surfactants, reaction-temperature and -time on the particle size of the product were investigated. NMC can be only obtained by using distilled water as a solvent, and of which the average particle size (APZ) is 106 nm. When sodium dodecyl sulfate and cetyl trimethyl ammonium bromide were used as surfactants, the APZ of the product is almost the same (about 100 nm). While nonylphenol polyoxyethylene ether was used, the APZ reaches up to 3.1 μm. The suitable reaction temperature and time for the preparation of NMC are 150℃ and 1-3 h respectively. Moreover, as toughening agent, the effect of both NMC and micro MC (MMC) on the performance of the toughened phenolic foam was investigated, and it was found that NMC is more effective rather than MMC in improving limiting oxygen index and flexural strength of the toughened foam.

Key words： organic polymer materials material synthesis nano melamine phosphate solvothermal method phenolic foam

收稿日期: 2013-11-13

基金资助:* 国家自然科学基金21174106 和U1205114/L11资助项目。

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https://www.cjmr.org/CN/10.11901/1005.3093.2013.857 或 https://www.cjmr.org/CN/Y2014/V28/I6/401

表1 PF泡沫配方表

图1 三聚氰胺氰尿酸盐的结构式

图2 三聚氰胺、氰尿酸和纳米MC的红外光谱

图3 微米MC和纳米MC的XRD图谱

图4 NMC的SEM像

图5 使用不同溶剂合成产物的粒径分布曲线

图6 使用不同表面活性剂合成产物的粒径分布曲线

图7 合成温度不同时产物的粒径分布曲线

图8 不同反应时间合成产物的粒径分布曲线

表2 PF泡沫的阻燃和力学性能

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