含能材料
含能材料
함능재료
ENERGETIC MATERIALS
2010年
1期
19-23
,共5页
有机化学%纳米固体超强酸%2,4,N-三硝基苯胺基乙酸%催化%硝化
有機化學%納米固體超彊痠%2,4,N-三硝基苯胺基乙痠%催化%硝化
유궤화학%납미고체초강산%2,4,N-삼초기분알기을산%최화%초화
organic chemistry%nanosolid superacid%2,4,N-trinitroanilinoacetic acid%catalysis%nitration
采用溶胶-凝胶法制备了新型的纳米固体超强酸催化剂TiO_2/SO_4~(2-),并用酸碱滴定、XRD、TEM进行了表征.结果表明,所研制的TiO_2/SO_4~(2-)催化剂为晶态纳米粒子,分散性较好,平均粒径为27 nm.以纳米固体酸TiO_2/SO_4~(2-)为催化剂,氯苯和氨基乙酸为原料直接合成了2,4,N-三硝基苯胺基乙酸(TNAA),收率为71.6%.最宜工艺条件: 氯苯为0.2 mol,催化剂为0.7 g,氨基乙酸为0.07 mol,硝酸为0.08 mol,反应温度为45 ℃,反应时间为3 h.催化剂焙烧温度600 ℃,催化剂重复使用8次仍保持较高活性.
採用溶膠-凝膠法製備瞭新型的納米固體超彊痠催化劑TiO_2/SO_4~(2-),併用痠堿滴定、XRD、TEM進行瞭錶徵.結果錶明,所研製的TiO_2/SO_4~(2-)催化劑為晶態納米粒子,分散性較好,平均粒徑為27 nm.以納米固體痠TiO_2/SO_4~(2-)為催化劑,氯苯和氨基乙痠為原料直接閤成瞭2,4,N-三硝基苯胺基乙痠(TNAA),收率為71.6%.最宜工藝條件: 氯苯為0.2 mol,催化劑為0.7 g,氨基乙痠為0.07 mol,硝痠為0.08 mol,反應溫度為45 ℃,反應時間為3 h.催化劑焙燒溫度600 ℃,催化劑重複使用8次仍保持較高活性.
채용용효-응효법제비료신형적납미고체초강산최화제TiO_2/SO_4~(2-),병용산감적정、XRD、TEM진행료표정.결과표명,소연제적TiO_2/SO_4~(2-)최화제위정태납미입자,분산성교호,평균립경위27 nm.이납미고체산TiO_2/SO_4~(2-)위최화제,록분화안기을산위원료직접합성료2,4,N-삼초기분알기을산(TNAA),수솔위71.6%.최의공예조건: 록분위0.2 mol,최화제위0.7 g,안기을산위0.07 mol,초산위0.08 mol,반응온도위45 ℃,반응시간위3 h.최화제배소온도600 ℃,최화제중복사용8차잉보지교고활성.
The new nanosolid superacid catalyst TiO_2/SO_4~(2-) was prepared by sol-gel method,and samples were characterized by acid base titration,XRD and TEM. Results show that the superfine solid TiO_2/SO_4~(2-) is nanocrystal with good dispersibility and its average size is 27 nm. With the catalyst TiO_2/SO_4~(2-),2,4,N-trinitroanilinoacetic acid(TNAA) was synthesized from chlorobenzene and glycine with yield of 71.6%. The optimum conditions are 0.2 mol chlorobenzene,and 0.7 g catalyst,and 0.07 mol glycine,and 0.08 mol nitric acid,and reaction time of 3 hours,and reaction temperature of 45 ℃. When calcined at 600 ℃,the activity of regeneration catalyst is restored mostly after regenerated eight times.
