|Table of Contents|

Synthesis and Characterization of Tetramethy 1,4-phenylene bis(methylene) bisphosphonate(PDF)

《南京师大学报(自然科学版)》[ISSN:1001-4616/CN:32-1239/N]

Issue:
2011年04期
Page:
55-59
Research Field:
化学
Publishing date:

Info

Title:
Synthesis and Characterization of Tetramethy 1,4-phenylene bis(methylene) bisphosphonate
Author(s):
Shi HongliLuo XuanWang DanZhou HaoZhi HuizhenYang Jinfei
School of Chemistry and Materials Science,Nanjing Normal University,Nanjing 210046,China
Keywords:
tetramethy 14-phenylene bis( methylene) bisphosphonateflame retardantsynthesischaracterization
PACS:
TQ265.1
DOI:
-
Abstract:
Tetramethy 1,4-phenylenebis( methylene) bisphosphonate,a new kind of highly efficient and halogen-free flame retardant,was synthesized by tetramethyl ammonium iodide catalyzed reactant of trimethyl phosphate with dichlorobenzyl. The best synthesis condition is that n( Trimethyl phosphate∶ dichlorobenzyl) = 2. 8∶ 1,at 130℃ for 6 h,with the amount of catalyst 3% of the total mass of reactants. The yield was up to 80%. Tetramethy 1,4 -phenylenebis( methylene) bisphosphonate was characterized by ESI-MS、1HNMR and IR spectral data. The thermal stability of Tetramethy 1, 4-phenylenebis ( methylene) bisphosphonate was examined by TGA.

References:

[1] Wang J S,Zhao H B,Ge X G,et al. Novel flame-retardant and antidripping branched polyesters prepared via-containing ionic monomer as end-capping agent [J]. Ind Eng Chem Res,2010,49: 4 190-4 196.
[2] Lu S Y,Lan H. Recent development in the chemistry of halogen-free flame retardant polymers [J]. Prog Polym Sci,2002, 27: 1 661-1 712.
[3] Gwilherm E,Krishnaji T,Franois C. Copper-mediated cross-coupling of 1,1-dibromo-1-alkenes with dialkyl phosphites: a convenient synthesis of 1-alkenylphosphonates [J]. Chem Commun,2011,47: 179-181.
[4] 蒋艾兵,程博闻,任元林. 二乙氧基丙烯酰胺甲氧基硫代磷酸酯( DAMT) 的合成及应用[J],应用化学, 2009, 26( 2) : 206-209.
[5] 欧育湘,李建军. 阻燃剂———性能、制造及应用[M]. 北京: 化学工业出版社, 2006: 161-208.
[6] Scientific date and heightened public safety concerns to drive growth in flame retardants [J]. Plastics Additives & Compounding, 2002( 4) : 28-31.
[7] Lim J C,Lee J H. Flame retardant thermoplastics resin composition: US,630524[P]. 2003-10-07.
[8] 郑虎,吴勇,温玲玲. 解热镇痛药———双膦酸酯化合物的合成[J]. 合成化学, 1999: 7( 4) 427-429.
[9] 吴明书,陈茹玉,黄有. 双膦酸及其酯类化合物的合成研究进展[J]. 有机化学, 2004, 24( 5) : 485-497.
[10] Zheng M,Bai F L,Li Y L,et al. Synthesis and characterization of a high-efficiency light-emitting alternating copolymer [J]. J Potym Sci A Potym Chem,1999,37: 2 587-2 594.
[11] Johnson R A,Smith H W. Phosphonic acid derivatives useful as antiinflammatory agents: WO 199210504( A2) [P]. 1992- 06-25.
[12] 虞燕华,陈志明,吴二明. 1,2 -双[双( 2-乙氧基乙基) 膦基]乙烷的合成改进[J]. 江苏药学与临床研究,2005,13 ( 6) : 13-14.
[13] 孙丽洁. 烷基取代膦酸二甲酯的合成与表征[J]. 辽宁大学学报: 自然科学版, 2004, 31( 1) : 78-80.
[14] 王丹,周浩,职慧珍,等. 无卤阻燃剂1,2-亚乙基双膦酸四甲酯的合成研究[J]. 精细化工, 2011, 28( 4) : 389-392.
[15] 张朝,胡宗超. 一锅法合成含氯二膦酸酯[J]. 贵州大学学报: 自然科学版, 2004, 21( 4) : 370-372.
[16] 金琼花,徐立军,吴界强,等. 手性四薄荷基亚甲基双膦酸酯的制备与性质表征[J]. 首都师范大学学报: 自然科学版, 2008, 29( 6) : 34-37.
[17] Xiang H F,Xu H Y,Wang Z Z,et al. Dimethyl methylphosphonate( DMMP) as an efficient flame retardant additive for the lithium-ion battery electrolytes[J]. Journal of Power Sources,2007,173: 562-564.
[18] 赵天增. 核磁共振氢谱[M]. 北京: 北京大学出版社,1983: 120-121.
[19] 卢林刚,陈淮思,曹飞,等. 新型无卤阻燃剂新戊二醇二焦磷酸酯的合成、晶体结构及热分解性能研究[J]. 化学学报, 2010, 68( 15) : 1 532-1 536.

Memo

Memo:
-
Last Update: 2013-03-21