火炸药学报
火炸藥學報
화작약학보
CHINESE JOURNAL OF EXPLOSIVES & PROPELLANTS
2015年
2期
35-38
,共4页
有机化学%N2O5%六硝基六氮杂异伍皍烷%绿色合成%2,6,8,12-四乙酰基-2,4,6,8,10,12-六氮杂四环-[5,5,0,03,11,05,9]十二烷%炸药
有機化學%N2O5%六硝基六氮雜異伍皍烷%綠色閤成%2,6,8,12-四乙酰基-2,4,6,8,10,12-六氮雜四環-[5,5,0,03,11,05,9]十二烷%炸藥
유궤화학%N2O5%륙초기륙담잡이오즉완%록색합성%2,6,8,12-사을선기-2,4,6,8,10,12-륙담잡사배-[5,5,0,03,11,05,9]십이완%작약
organic chemistry%N2 O5%2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane%green synthesis%2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo [5,5,0,03,11 05,9 ]dodecane%explosive
以2,6,8,12-四乙酰基-2,4,6,8,10,12-六氮杂四环-[5,5,0,03,11,05,9]十二烷(TAIW)为原料,采用 N2 O5/HNO3为硝化剂硝解 TAIW 制备六硝基六氮杂异伍皍烷(CL-20)。通过系统研究 N2 O5/HNO3硝解 TAIW 的加料方式、温度、料比、反应时间、稀释用水量等因素对反应收率和纯度的影响,找出了最佳反应条件:反应温度60~80℃,反应时间7 h,m(TAIW)∶m (N2 O5)∶V(HNO3)=3 g∶4 g∶15 mL,后处理时稀释用水量20 mL,CL-20收率为82.34%,纯度为98.29%。当以质量分数10%的 CF3 SO3 H/树脂为催化剂时,收率提高至87.35%,纯度基本不变,且催化剂的回收率达到99.15%。该方法避免硫酸的使用,减轻了废酸污染,具有较强的工业化应用前景。
以2,6,8,12-四乙酰基-2,4,6,8,10,12-六氮雜四環-[5,5,0,03,11,05,9]十二烷(TAIW)為原料,採用 N2 O5/HNO3為硝化劑硝解 TAIW 製備六硝基六氮雜異伍皍烷(CL-20)。通過繫統研究 N2 O5/HNO3硝解 TAIW 的加料方式、溫度、料比、反應時間、稀釋用水量等因素對反應收率和純度的影響,找齣瞭最佳反應條件:反應溫度60~80℃,反應時間7 h,m(TAIW)∶m (N2 O5)∶V(HNO3)=3 g∶4 g∶15 mL,後處理時稀釋用水量20 mL,CL-20收率為82.34%,純度為98.29%。噹以質量分數10%的 CF3 SO3 H/樹脂為催化劑時,收率提高至87.35%,純度基本不變,且催化劑的迴收率達到99.15%。該方法避免硫痠的使用,減輕瞭廢痠汙染,具有較彊的工業化應用前景。
이2,6,8,12-사을선기-2,4,6,8,10,12-륙담잡사배-[5,5,0,03,11,05,9]십이완(TAIW)위원료,채용 N2 O5/HNO3위초화제초해 TAIW 제비륙초기륙담잡이오즉완(CL-20)。통과계통연구 N2 O5/HNO3초해 TAIW 적가료방식、온도、료비、반응시간、희석용수량등인소대반응수솔화순도적영향,조출료최가반응조건:반응온도60~80℃,반응시간7 h,m(TAIW)∶m (N2 O5)∶V(HNO3)=3 g∶4 g∶15 mL,후처리시희석용수량20 mL,CL-20수솔위82.34%,순도위98.29%。당이질량분수10%적 CF3 SO3 H/수지위최화제시,수솔제고지87.35%,순도기본불변,차최화제적회수솔체도99.15%。해방법피면류산적사용,감경료폐산오염,구유교강적공업화응용전경。
2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20)was prepared via nitrolysis of 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo [5,5,0,03 ,11 05 ,9 ]dodecane (TAIW)as starting material and N2 O5/HNO3 as nitrating agent.Through studying the effect of the reaction conditions such as filling type for nitrolysis of TAIW with N2 O5/ HNO3 ,temperature,the amount of HNO3 and N2 O5 ,reaction time,the amount of the diluted water on the yield and purity of CL-20,the optimal reaction conditions are determined as:reaction temperature 60-80 ℃,reaction time 7 h,the ratio of m(TAIW)∶m(N2 O5 )∶V (HNO3 )of 3 g∶4 g∶15 mL,and addition of diluted water in the post process 20 mL,at this time,the yield of CL-20 is 82.34% ,and its purity is 98.29%.When 10%CF3 SO3 H/resin is used as catalyst,the yield is up to 87.35% ,its purity remains basically unchanged and the recovery rate of catalyst reaches to 99.15%.This method can avoid the use of sulfuric acid and reduce the pollution of the waste acid with strong industrial application prospect.