[1]周浩,王丹,张士磊,等.双季戊四醇二亚磷酸酯阻燃剂的合成[J].南京师范大学学报(工程技术版),2010,10(02):048-52.
 Zhou Hao,Wang Dan,Zhang Shilei,et al.Synthesis of Fire Retardants of Dipentaerythritol Diphosphonate Ester[J].Journal of Nanjing Normal University(Engineering and Technology),2010,10(02):048-52.
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双季戊四醇二亚磷酸酯阻燃剂的合成
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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:
10卷
期数:
2010年02期
页码:
048-52
栏目:
出版日期:
2010-02-01

文章信息/Info

Title:
Synthesis of Fire Retardants of Dipentaerythritol Diphosphonate Ester
作者:
周浩 王丹 张士磊 职慧珍 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):
Zhou HaoWang DanZhang ShileiZhi HuizhenYang Jinfei
School of Chemistry and Environmental Science,Nanjing Normal University,Nanjing 210097,China
关键词:
双季戊四醇 亚磷酸三苯酯 酯交换 二亚磷酸酯 阻燃剂
Keywords:
d ipentaerythrito l tripheny lphosph ite ester exchange diphosphonate fire reta rdant
分类号:
TQ265.1
摘要:
以双季戊四醇(DPE)、亚磷酸三苯酯(TPP)为原料,氢氧化钠为催化剂,通过酯交换反应得到双季戊四醇二亚磷酸酯阻燃剂.用正交法讨论了原料物质的量之比、反应温度、反应时间、催化剂种类和用量对反应的影响,确定了反应的最佳条件:催化剂为氢氧化钠,其用量为反应物总质量的1%,n(P(OPh)3)∶n(C10H22O 7)为2.06∶1,反应温度为100℃~110℃,反应时间为10 h,双季戊四醇二亚磷酸酯收率为86.3%.采用红外吸收光谱和元素分析初步证实了产品的结构.
Abstract:
Dipentaery thrito l cyc lic phosphonate ester was synthesized from d ipentaerythrito l( TPE ) and tr ipheny lphos ph ite( TPP) in the presence of sod ium hydrox ide cata lyst by a step of ester exchang e reaction. The e ffects o f process pa  rame ters, such as m o lar ratio, reaction temperature, reaction tim e and cata ly st on the y ie ld w ere studied respectively from o rthogona l experim ents. The su itab le synthesis conditions we re de fined as fo llow s: sodium hydrox ide is the suitable ca talyst, its dosage is 1% of the am ount of a ll reactan t, them o la r ratio of triphenylphosph ite and dipentaerythrito l is 2. 06 :1, the reaction tem pe rature is 100℃  ~ 110℃  , and the reaction tim e is 10 hours. On the above cond itions, the syn  thesis produc tiv ity is 86. 3%. The structure of the produc t was confirm ed by IR and EA respec tive ly.

参考文献/References:

[ 1] 欧育湘. 实用阻燃技术[M ]. 北京: 化学工业出版社, 2002. Ou Yux iang. Practical F lame Re tardan t Techn iques[M ]. Be ijing: Chem ical Industry Press, 2002. ( in Ch inese)
[ 2] Verkade J G, Reyno ids L J. The synthesis o f a nove l ester o f phorphous and o f arsen ic[ J] . Journal o fO rganic Chem istry, 1960, 25: 633.
[ 3] Char les F B, Irv ing G, N iagara F. Pentaerythriol phosph ites: USA, 3310609[ P] . 1967.
[ 4] Char les F B, Irv ing G, N iagara F. Pentaeryt hriol phosphates as flame reta rdants in fo am s and e lastom ers: USA, 3412025 [ P]. 1968.
[ 5] 孙春梅, 龚铮, 吴荣梁, 等. 三季戊四醇亚磷酸酯阻燃剂的合成及应用研究[ J]. 功能高分子材料, 2005, 6( 2) : 260-264. Sun Chunm e,i Gong Zheng,W u Rong liang, et a.l Study on the prepara tion o f tripentaery thr ito l phosphite intumescent flam e re  tardant and its app lication in epox y resins[ J]. M ate rials o f Functional Po lyme rs, 2005, 6( 2): 260-264. ( in Ch inese)
[ 6] M iche l Dem arcq. Pho spho rus derivatives of pentae rythr ito l monobrom ohydrin: USA, 4169118[ P] . 1979.
[ 7] 朱春华, 陈红梅, 吴德清. 涤纶织物浸扎用阻燃剂环状磷酸酯的合成[ J] . 合成纤维工业, 2008, 31( 6): 23-26. Zhu Chunhua, Chen H ongme ,iW u Deqing. Synthesis o f cy clic pho sphate flam e re tardant for padding process o f PET fabr ic[ J]. China Synthetic Fiber Industry, 2008, 31( 6): 23-26. ( in Chinese)
[ 8] 苏秋芳. 三乙胺催化合成2??羟丙基甲醚[ J]. 精细化工中间体, 2004, 34( 4): 49-51. Su Q iu fang. Synthesis of 1 m ethoxy 2 propano l w ith tr iethy lam ine ca talyst[ J]. F ine Chem ical Interm ediates, 2004, 34( 4): 49-51. ( in Chinese)
[ 9] 郑燕升, 栗晖, 李军生, 等. 三乙胺催化合成维生素E 乙酸酯的研究[ J]. 广西工学院学报, 2006, 17( 3): 33-35. Zheng Yansheng, LiH u,i Li Junsheng, et a.l Study on the ca talytic synthesis o f v itam in eacetate by triethy lam ine[ J]. Journal o f Guangx iUniversity of Techno logy, 2006, 17( 3): 33-35. ( in Ch inese)
[ 10] 严慧, 杨智中, 杨锦飞. 环状磷酸酯阻燃剂An tiblaze的合成[ J]. 南京师范大学学报: 工程技术版, 2009, 9( 1) : 53-56. Yan H u,i Yang Zhizhong, Yang Jinfe .i Synthes is o f fire retardant cyclic phosphona te este r[ J]. Journal of Nanjing No rm al Un ive rs ity: Eng ineer ing and Techno logy Ed ition, 2009, 9( 1): 53-56. ( in Ch inese)
[ 11] 梁诚. 亚磷酸酯类抗氧剂的现状与发展[ J]. 塑料助剂, 2005( 5): 13-19. L iang Cheng. Techno log ical prog ress of phosphite antiox idan t[ J]. Plastic Additives, 2005( 5): 13-19. ( in Ch inese)
[ 12] 张学岭, 胡应喜. 二亚磷酸二(十四醇) 季戊四醇酯的合成[ J]. 北京石油化工学院学报, 2007, 12( 4): 20-23. Zhang Xueling, H u Y ingx .i Synthesis of B is( 1 tetradecanol) pen tae ry thr ito l diphosphite [ J]. Journa l o f Be ijing Institute o f Petro chem ica lTechnology, 2007, 12( 4): 20-23. ( in Chinese)

备注/Memo

备注/Memo:
基金项目: 江苏省科技厅科技攻关项目( BE2007050 ) . 通讯联系人: 杨锦飞, 教授, 研究方向: 阻燃剂及药物中间体的合成. Em ail:yangj infei@ n jnu. edu. cn
更新日期/Last Update: 2013-04-02