[1]黄小冬,顾慧丹,黄东平,等.亚磷酸三异癸酯的合成条件研究[J].南京师范大学学报(工程技术版),2005,05(04):068-71.
　HUANG Xiaodong,GU Huidan,HUANG Dongping,et al.Study on Synthesis Conditions of Triisodecyl Phosphite Ester[J].Journal of Nanjing Normal University(Engineering and Technology),2005,05(04):068-71.
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亚磷酸三异癸酯的合成条件研究
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南京师范大学学报（工程技术版）[ISSN:1006-6977/CN:61-1281/TN]

卷:
05卷
期数:
2005年04期
页码:
068-71
栏目:
出版日期:
2005-12-30

文章信息/Info

Title:
Study on Synthesis Conditions of Triisodecyl Phosphite Ester
作者:
黄小冬;顾慧丹;黄东平;杨锦飞;
南京师范大学化学与环境科学学院, 江苏南京210097
Author(s):
HUANG Xiaodong; GU Huidan; HUANG Dongping; YANG Jinfei
School of Chemistry and Environmental Science,Nanjing Normal University,Jiangsu Nanjing 210097,China
关键词:
亚磷酸三异癸酯;  异癸醇;  三氯化磷;  吡啶;  苯;  合成
Keywords:
tr iisodecy l phosphite ester;  isodecy l alcoho ; l phosphorus tr ich lor ide;  py ridine;  benzene;  synthesis
分类号:
O627.51
摘要:
由异癸醇和三氯化磷反应制得亚磷酸三异癸酯.通过对比实验确定了以吡啶为缚酸剂、苯为溶剂.采用正交试验法确定适宜的工艺条件为:反应温度为60℃,溶剂用量约为异癸醇质量的3倍,滴加时间控制在90 m in,反应时间为1.5 h,异癸醇和三氯化磷的物质的量之比为3.1∶1.在此条件下,合成产率可以达到96.8%,产品质量达到国外同类产品的指标.产品经红外、核磁光谱表征.
Abstract:
Tr iisodecy l phosph ite ester is synthesized w ith isodecyl alcoho l and PC l3 by using the d irec t esterification m ethod. It is de term ined w ith the com par ison m e thod that py rid ine and benzene are used as theHC l acceptor and the so lvent, respec tive ly. W ith an orthogonal experim entm ethod, the su itable synthesis cond itions are de fined as fo llow s: the reac tion tem pe ra ture: 60℃ , the so lvent quantity: 3 tim es the m ass of isodecy l a lcoho,l the dropw ise tim e: 90 m in, reaction tim e: 1. 5 h, them o lar ratio of isodecy l a lcoho l and PC l3: 3. 1：1. Under the above cond itions, synthe-t ic productiv ity can reach 96. 8%. The qua lity o f the product can reach the indexes of the oversea products.

参考文献/References:

[ 1] W illiam Dav id Phillips. Lubr icant compositions con taining sulfur and phosphorus: WO, 2004096959 [ P]. 2004-11- 11.
[ 2] Thom as Deforth, Gera rdM ignan .i Christian Pus ine r.i U se o f po lysilox anes hav ing antiox idant g roups for stabilizing o f po lym ers: WO, 2002006381 [ P]. 2002-03-21.
[ 3] Dona ld R S tevenson, Thomas C Jenn ings, M ark E H arr, et al. Phosph ite ester add itive com po sitions: US, 2004183054 [ P]. 2004-09-23.
[ 4] Robert C Blosser, John F Gurcsik, Char les E W h ite. Process fo r m ak ing phosphite esters from tr ipheny l phosphite and alcoho ls in the presence of sod ium phenate catalyst: EP, 553984 [ P]. 1993-08-04.
[ 5] Koso lapoff G M, M a ier L. Org an ic Phospho rus Compounds [M ]. New York: John W iley and Sous, 1972: 23- 27.

备注/Memo

备注/Memo:
作者简介: 黄小冬( 1978-) , 硕士研究生, 主要从事有机合成与阻燃剂方向的学习和研究. E-ma il: reatum@ 126. com
通讯联系人: 杨锦飞( 1965-) , 教授, 主要从事有机化学和阻燃剂及药物中间体合成的教学与研究. E-m ail: yangjin fei@n jnu. edu. cn
更新日期/Last Update: 2013-04-29