摘要
目的 采用溶胶凝胶法对密胺甲醛树脂微胶囊红磷(MRP)进行改性,并探究最佳工艺条件,以加强其使用性能。方法 以正硅酸乙酯(TEOS)为原料,选取TEOS添加量为工艺条件,采用溶胶凝胶法改性MRP,制备硅凝胶-密胺甲醛树脂双层包覆微胶囊红磷(Si-MRP)。利用傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)及X射线光电子能谱(XPS)对Si-MRP形态及包覆效果进行表征,并进行吸湿率测定、热稳定性分析及安定性测定。结果 采用溶胶凝胶法在MRP表面引入一层硅凝胶结构,实现了红磷颗粒的硅凝胶-密胺甲醛树脂双层包覆。TEOS添加量对样品形态及包覆率有一定影响,随着TEOS添加量的增多,Si-MRP形态从光滑层状结构向颗粒堆积结构过渡,硅凝胶包覆率由97.5%降至93.6%。硅凝胶结构提高了MRP的热稳定性,降低了吸湿率,增强了样品安定性。当TEOS与待改性MRP样品质量比为1:2.5时,制备的Si-MRP样品的着火点相对于MRP提高80 ℃,10 d后吸湿率降至3.7%,摩擦感度降至14%。结论 采用溶胶凝胶法可对MRP实现有效包覆,经硅凝胶包覆后的样品使用性能得到进一步提高。
Abstract
The work aims to improve performance of melamine-formaldehyde resin microencapsulated red phosphorus (MRP), modify it in sol-gel method, and study the optimum technological conditions. With tetraethoxysilane (TEOS) as precursor and TEOS additive amount as process conditions, silica gel-MF resin double layered microencapsulated red phosphorus (Si-MRP) was prepared via sol-gel modification. Surface morphology and coating effect of Si-MRP were characterized by FT-IR, SEM and XPS. Meanwhile, moisture rate, thermal stability and sensitivity of the samples were also tested. A layer of silica gel structure was introduced on the surface of MRP in sol-gel method successfully to coatsilica gel-MF resin double layered microencapsulated red phosphorus (Si-MRP). The morphology and coating ratio of Si-MRP was influenced by the TEOS additive amount. With the increase of TEOS, surface morphology of Si-MRP transformed from stratiform structure to particle accumulation structure, and the coating ratio decreased from 97.5% to 93.6%. The silica gel structure enhanced thermal and mechanical stability of MRP, and decreased moisture rate. Provided with TEOS-MRP mass ratio of 1:2.5, ignition temperature of Si-MRP prepared increased by 80 ℃ compared with MRP, and the moisture rate and friction sensitivity decreased to 3.7% and 14%, respectively. MRP can be microencapsulated effectively in sol-gel method, and performance of the samples can be further improved after microencapsulation.
关键词
微胶囊;溶胶凝胶法;硅凝胶;密胺甲醛树脂;红磷;安定性
Key words
microcapsule; sol-gel; silica gel; melamine-formaldehyde resin; red phosphorus; stability
程晨, 杜仕国, 鲁彦玲, 刘献杰.
溶胶凝胶法改性密胺甲醛树脂微胶囊红磷[J]. 表面技术. 2018, 47(9): 74-80
CHENG Chen, DU Shi-guo, LU Yan-ling, LIU Xian-jie.
Melamine-formaldehyde Resin Microencapsulated Red Phosphorus Modified in Sol-Gel Method[J]. Surface Technology. 2018, 47(9): 74-80
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