第25卷第2期 2017年6月
油化工学
北京石
院学报
Journal of Beijing Institute of Petrochemical Technology
文章编号：1008-2565(2017)02-0019-06
Vol.25No.2 Jun.2017
4ZnO·B,O3：H2O的微波水热合成与表征
张丽芳，王岑晨，黄佟霞，王宗霜，张璐，刘霞
（北京石油化工学院化学工程学院，北京102617）
摘要：硼酸锌是一种新型高效无机阻燃剂。为了优化制备硼酸锌的反应条件并研究其阻燃性能，以七水硫酸锌和酬砂为原料，采用微波水热法合成硼酸锌（4ZnO·B,O，·H,O)，通过XRD,SEM、TG一DTA进行表征并对其阻燃性能进行测试，优化后的实验条件为：锌与翻砂物质的量的比为1：1.2，固液质量比为1：10，140下微波水热反应时间为10min。该条件下所得硼酸锌的失水温度高于415C，形貌呈不规则片状，厚度约为100nm：添加质量分数为10%的该样品于木屑中，400℃时的残碳率与纯木屑样品相比高约27%，在制备硼酸锌过程中，漆加硬脂酸钠或含有硬脂酸钠的复配修饰剂后，改性效果均较好，所得样品亲油疏水，且样品形貌有变化，其中同时添加硬脂酸钠和聚乙二醇所得样品为分散较均匀的纳米棒，直径为50～80nm，
关键词：硼酸锌；微波水热法；改性；阻燃性能
中图分类号：0613.8+1
文献标志码：A
DOl:10.12053/j.issn.1008-2565.2017.02.005
Microwave-hvdrothermalSvnthesisandCharacterization
of4ZnO:B,O3:H,0
ZHANG Lifang+ WANG Cenchen, HUANG Tongxia,
WANG Zongshuang+ ZHANG Lu, LIU Xia
(College of Chemical Engineering, Beijing Institute of Petro-chemical Technology, Beijing 102617, China) Abstract: Zinc borate is a new and efficient inorganic fire retardant. Study of the optimal reaction conditions for preparing the zinc borate and its flameretardant property is of vital significance. In this research, zinc sulfate heptahydrate and borax were used as raw materials to synthesize zinc borate 4ZnO · B,O,2H,O via the microwave hydrothermal method. It was analyzed by XRD. SEM, TG-DTA, and its flame-retardant property was tested. The optimized experimental conditions are as follows: the molar ratio of zinc sulfate and borax is 1 : 1. 2, the solid-liquid mass ratio is 1 : 10, and the microwave hydrothermal reaction time is 10 min at 14o C. Under these conditions, the resultant zinc borate has a dehydration temperature higher than 415 'C, flaky morphology and sample thickness of about 1o0 nm. With 1o% of the sample in the wood, the char yield at 400 C is about 27% higher than that of pure wood sample. After adding sodium stearate or modifying agent containing sodium stearate complex into the reaction process, the modification effects were good with the resulting sample lipophilic and the sample morphology changed. By adding sodium stearate and polyethylene glycol, the resulting samples were dispersed more uniform nanorod and the diameter was about 50~80 nm.
Key words: zinc borate; microwave hydrothermal method; modified; flame retardant 收稿日期：2016-11-26
作者简方数据(1971—），女，本科，实验师，研究方向为精细化学品的合成，E-mail：zhanglifang@bipt.edu.cn，