纳米固体酸的制备及2,4,N-三硝基苯胺基乙酸的合成

采用溶胶-凝胶法制备了新型的纳米固体超强酸催化剂TiO2/SO42-,并用酸碱滴定、XRD、TEM进行了表征。结果表明,所研制的TiO2/SO24-催化剂为晶态纳米粒子,分散性较好,平均粒径为27nm。以纳米固体酸TiO2/SO24-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0.2mol,催化剂为0.7g,氨基乙酸为0.07mol,硝酸为0.08mol,反应温度为45℃,反应时间为3h。催化剂焙烧温度600℃,催化剂重复使用8次仍保持较高活性。

Preparation of Nanosolid Superacid and Synthesis of 2,4,N-Trinitroanilinoacetic Acid Directly

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.