硅氮磷协同阻燃剂的合成及其阻燃性能.pdf

石油化工
2015年第44卷第10期
PETROCHEMICAL TECHNOLOGY
1229
硅氮磷协同阻燃剂的合成及其阻燃性能
杨海军,王度林
(苏州科技学院化学生物与材料工程学院,江苏苏州215009)
[摘要j以三羟乙基异氧尿酸酯(赛克)、二甲基二氯硅烷( DMDCS)和1ー氧代ー1-磷杂-4-羟甲基-2,6,7-三氧杂双环[2,2.2
辛烷(PEPA)为原料,合成多元素协同阻燃剂异氰尿酸三{2-[二甲基(1-氧代ー1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷基
甲氧基)硅氧基]乙基}醋( TPOSC),探讨反应温度对HC气体放完所需时间的影响和反应物配比等对产物收率的影响。实验
结果表明,以二氧六环为溶剂,在(赛克):n( DMDCS):m(PEPA)=10:3.0:3.3、第一步在70℃反应7h、第二步在90℃
反应8h的最优工艺条件下,收率可达92.1%。FTIR、" HNMR、热重分析等表征结果显示,合成的产物结构与目标产物一致,
产物有较好的热稳定性,对聚丙烯阻燃成炭的效果好,且与三聚氰胺氰尿酸盐复配使用时具有很好的阻燃协同增效性。
L关键词三羟乙基异氰尿酸酯;二甲基二氯硅烷;阻燃剂;硅氮磷协同
[文章编号]1000-8144(2015)10-1229-05
[中图分类号]TQ314.248
[文献标志码
Synthesis and Flame Retardance of a Silicon, Nitrogen
Phosphorus Synergistic Flame Retardant
Yang Haijun, Wang Yanlin
(School of Chemistry Bioligy and Material Engineering, Suzhou University of Science and Technology
Suzhou Jiangsu 215009, China)
I Abstractj A multi-element synergistic flame retardant, 1, 3, 5-tris2-[ dimethyl(1-oxo
phospha-2, 6, 7-trioxabicyclol2.2.2] octallkyl-4-methyloxy siloxy] ethyl] isocyanurate(TPOSC
was synthesized from 1, 3, 5-tris(2-hydroxyethyl )isocyanurate, dimethyldichlorosilane and 1-0xo
1-phospha-4-hydroxymethyl-2, 6, 7-trioxabicyclo[2. 2. 2 octane(PEPA) and was characterized by
means of FTIR, H NMR, and TG/DTA. The effect of reaction temperature on the reaction time
when Hcl was completely released and the influence of raw material ratio on the product yield were
investigated. It was showed that, under the optimal conditions of dioxane as solvent, n(1, 3, 5-tris(2-
hydroxyethyl)cyanurate): n(dimethyldichlorosilane): n(PEPA)1.0: 3.0: 3.3, 70 C and 7 h for
the first step reaction, and 90 C and 8 h for the second step reaction, the product yield could reach
92.1%o. The characterization results verified the structure off the product. The product has excellent
thermal stability and high flame-retardance efficiency for polypropylene(PP). Besides, when it was
mixed with melamine cyanurate and was applied to PP, high synergistic flame-retardance efficiency
was found
Keyword 1, 5-tris(2-hydroxyethyl)isocyanurate; dimethyldichlorosilane; flame retardant
silicon, nitrogen, phosphorus synergism
自20世纪90年代以来,阻燃技术及阻燃行业无卤阻燃剂的研究与开发13。但上述无卤阻燃剂
都在快速地发展。在实际应用中卤系阻燃剂所存在大多存在阻燃效率低、添加量大及劣化高分子材料
的弊端促进了无卤阻燃剂,如磷系、氮系和硅系等的力学性能等缺点,因此其发展也很缓慢4。现
收稿日期]2015-05-08;[修改稿日期]2015-06-2
[作者简介]杨海军(1990-),男,江苏省泰兴市人,硕士生。联系人:王彦林,电话0512-68418430,电邮wangyanlinsz@l63.com。