广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2011年
20期
61-63
,共3页
薛宇鹏%郝冬梅%林倬仕%陈涛%尹亮%陈崇伟%王幸宜
薛宇鵬%郝鼕梅%林倬仕%陳濤%尹亮%陳崇偉%王倖宜
설우붕%학동매%림탁사%진도%윤량%진숭위%왕행의
苯氧基环磷腈%六氯环三磷腈%苯酚%合成%后处理
苯氧基環燐腈%六氯環三燐腈%苯酚%閤成%後處理
분양기배린정%륙록배삼린정%분분%합성%후처리
phenoxy cyclotriphosphazene%hexachlorocyclotriphosphazene%phenol%synthesis%post-treatment
苯氧基环三磷腈是一种重要的磷腈化合物,而苯氧基环磷腈(PCPZ)的制备会产生大量的副产物和过量的苯酚钠存在,使得合成实验的后处理较复杂且得很难得到纯度很高的产物。利用苯酚钠和六氯环三磷腈制备的苯氧基环三磷腈,根据产物易溶于四氢呋喃但难溶于水这一特点,找到了一种很简单的方法,使产物在大量水中结晶析出。这个方法操作方便,通过红外光谱、核磁共振、X衍射、高效液相色谱、热分析和凝胶渗透色谱表明得出的产物收率高于97%,纯度达100%,是一种很理想的后处理方法。
苯氧基環三燐腈是一種重要的燐腈化閤物,而苯氧基環燐腈(PCPZ)的製備會產生大量的副產物和過量的苯酚鈉存在,使得閤成實驗的後處理較複雜且得很難得到純度很高的產物。利用苯酚鈉和六氯環三燐腈製備的苯氧基環三燐腈,根據產物易溶于四氫呋喃但難溶于水這一特點,找到瞭一種很簡單的方法,使產物在大量水中結晶析齣。這箇方法操作方便,通過紅外光譜、覈磁共振、X衍射、高效液相色譜、熱分析和凝膠滲透色譜錶明得齣的產物收率高于97%,純度達100%,是一種很理想的後處理方法。
분양기배삼린정시일충중요적린정화합물,이분양기배린정(PCPZ)적제비회산생대량적부산물화과량적분분납존재,사득합성실험적후처리교복잡차득흔난득도순도흔고적산물。이용분분납화륙록배삼린정제비적분양기배삼린정,근거산물역용우사경부남단난용우수저일특점,조도료일충흔간단적방법,사산물재대량수중결정석출。저개방법조작방편,통과홍외광보、핵자공진、X연사、고효액상색보、열분석화응효삼투색보표명득출적산물수솔고우97%,순도체100%,시일충흔이상적후처리방법。
Phenoxy cyclotriphosphazene was one of the most important phosphazene compounds,but for the existence of by-products and excessive sodium phenolate,the post-treatments for synthesis of phenoxy cyclotriphosphazene were complicated and it was hard to obtain products with high purity.Phenoxy cyclotriphosphazene was prepared with sodium phenolate and hexachlorocyclotriphosphazene.Since phenoxy cyclotriphosphazene could dissolve in THF,but could not in water.The product was poured into a beaker with a lot of water and phenoxy cyclotriphosphazene was precipitated.The product was analyzed by FTIR,NMR,XRD,HPLC,TGA,DSC and GPC.The yield was higher than 97% and the purity was 100%.