全氟二(2,5,8-三甲基-11-氟磺酰基-3,6,9-三氧杂十一酰基)过氧化物的合成

Synthesis of the Perfluorobis(11-fluorosulfonyl-2,5,8-trimethyl-3,6,9-trioxaundecanoyl) Peroxide

以全氟-2,5,8-三甲基-11-氟磺酰基-3,6,9-三氧杂十一酰氟、氢氧化钠和双氧水为原料,全氟-2-甲基四氢呋喃和全氟-2-乙基四氢呋喃的混合物为溶剂,合成了1种新的全氟酰基过氧化物:全氟二(2,5,8-三甲基-11-氟磺酰基-3,6,9-三氧杂十一酰基)过氧化物(FAP),用红外光谱法对产物结构进行了表征,测定了FAP分解反应的动力学数据,并推算出较低温度下的分解反应速率常数和半衰期。通过正交实验得到最佳条件为:氢氧化钠的浓度为6mol/L,n(H2O2)∶n(NaOH)=1.4∶1,反应温度-8℃,反应时间30min。FAP的平均收率为52.6%,可在-30℃以下较长时间贮存。

A new perfluorodiacyl peroxide, named perfluorobis(11-fluorosulfonyl-2,5,8-trimethyl-3,6,9-trioxaundecanoyl) peroxide was synthesized with perfuloro-11-fluorosulfonyl-2,5,8-trimethyl-3,6,9-trioxaundecanoyl fluoride, sodium hydroxide and hydrogen peroxide. The structure of the product was characterized with IR. The reaction conditions were optimized through orthogonal method and the yield of the product finally meets the value of the analog reported.