聚合型含硫有机膦阻燃剂的制备及其应用.pdf

石油化工
2012年第41卷第7期
PETROCHEMICAL TECHNOLOGY
811
聚合型含硫有机驎阻燃剂的制备及其应用
王彦林,张艳丽,纪孝熹,刁建高,王冬军
(苏州科技学院化学与生物工程学院,江苏苏州215009)
摘要」在无溶剂条件下,以苯基硫代酰二氯、10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂非(DOPO-HQ)为原料,合成了
一种聚合型含碗有机膦阻燃剂聚苯棊硫代酸(10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂菲)酯( PDPTP)。考察了反应时间
和反应温度对收率的影响,确定了宜的反应条件为:n(苯基硫代膦毗二氯):れ(DOPO-HQ)=1:1,160℃下恒温h,240
℃下反应4h。在此条件下, PDPTP收率为990%。采用FTIR、HNMR、元素分析等方法对产物结构进行了表征,并采用TG-
DTA方法对其热稳定性进行了分析。表征结果显示,所合成的化合物为目标产物 PDPTP,热分解温度为270。利用氧指数
测定仪测试 PDPTP的阻燃性能时发现, PDPTP对聚对苯二甲酸丁二醇具有较好的阻燃性。
关键词]苯基硫代铣二氯;无溶剂法;聚苯基硫代隣酸(10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂菲)脂;聚合型含硫有
机膦阻燃剂
文章编号]10008144(2012)07-0811-04
中图分类号jTQ314,248
[文献标识码]A
Preparation and Application of a Polymeric Sulfur-containing
Organophosphorus Flame Retardant
Wang Yanlin, Zhang Yanli, i Xiaoxi, Diao Jiangao, Wang Dongjun
College of Chemistry and Biological Engineering, Suzhou University of Science and Technology, Suzhou Jiangsu 215009, China)
Abstract J Poly-phenyl-phosphonothioic acid(10-(2, 5-dihydroxypheny1)-9-xa-10-phosphoryl
hybrid-philippines)ester(PDPTP )as a polymeric sulfur-containing organophosphorus flame retardant
was synthesized from phenylthiophosphonic dichloride and 10-(2, 5-dihydroxyphenyl)-9-xa-10
phosphoryl hybrid-philippines(dopo-hq)by a solvent-free method. The effect of reaction time and
reaction temperature on the yield of PDPTP was studied. Under the optimal reaction conditions of
n(phenylthiophosphonic dichloride): n(DOPO-HQ)1: 1, reaction firstly at 160 C for 1 h and then
at 240 C for 4 h, the yield of PDPTP can reach 99.0%0. The chemical structure of the product was
characterized by means of FTIR, H NMR and elementary analysis. The results show that the product
IS PDPTP. Its thermal degradation behavior and flame retardancy were investigated by means of TG
DTA and oxygen index analyzer And the results indicate that its decomposition temperature is 270 C
and it has excellent flame retardancy for polybutylene terephthalate
I Keywords] phenylthiophosphonic dichloride; solvent-free method; poly phenyl phosphonothioic
acid(10-(2, 5-dihydroxyphenyl)-9-xa-10-phosphoryl hybrid-philippines) ester; polymeric sulfur
containing organophosphorus flame retardant
广义的有机膦阻燃剂以僯酸酯居多,并多为研究热点-。
液体,存在耐热性较差、挥发性大、发烟量大、
本工作在无溶剂条件下,合成了一种聚合型
与聚合物相容性差等缺点。因此,急需开发热含硫有机膦阻燃剂聚苯基硫代膦酸(10-(2,5
稳定性好、相对分子质量大、与材料相容性好、含
磷量高、低烟、无毒和具有C一P键的有机瞵阻燃
[收稿日期]2012-01-19;[修改稿日期]2012-03-26
作者简介]王度林(1957ー),男,河南省开封市人,大学
剂26。多元素协同型有机驎阻燃剂由于能赋予材
教授,电话0512-68418430,电邮wangyanlinsz(163.com
料更好的加T性能,已成为当前阻燃剂行业的一个[基金项目]苏州市应用基础研究计划项日(SYJG0928)。