Mn_3O_4的室温制备及其对高氯酸铵热分解的催化性能
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摘要
以Mn Cl_2、Na OH、H_2O_2为原料,以十二烷基苯磺酸钠(SDBS)为分散剂,制备纳米Mn_3O_4。通过XRD表征产物。采用差示扫描量热法(DSC)和热重分析(TG)考查纳米Mn_3O_4对高氯酸铵(AP)热分解的催化作用。结果表明:在Mn Cl_2(0.25mol/L)用量100m L的条件下,制备纳米Mn_3O_4的最佳工艺为:Na OH(0.5mol/L)100m L;H_2O_2(2.5mol/L)14m L;SDBS(0.025mol/L)6m L;室温下,制备前驱物,对前驱物的热处理温度为300℃,热处理时间为2h,该条件下制备出的纳米Mn_3O_4的产率为77.50%,粒径为14.52nm。纳米Mn_3O_4对AP热分解的催化活性很高,可使AP的高温热分解温度显著降低,分解放热量显著增加,粒径越小其催化活性越高。
Mn_3O_4 nanocrystalline was prepared by MnCl_2,NaOH,and H_2O_2 as the starting materials and surfactant sodium dodecyl benzene sulfonate?( SDBS) as dispersant,and it was characterized by X-raydiffraction( XRD). The catalytic properties of. Mn_3O_4 nanocrystalline on the thermal decomposition of ammonium perchlorate( AP) were investigated by differential scanning calorimetry( DSC) and thermogravimetric analysis( TG). The experimental results indicated that the optimum conditions for preparing Mn_3O_4 nanocrystalline are as follows: At room temperruture,precursor is prepared by NaOH( 0. 5mol /L) 100 mL,H_2O_2( 2. 5mol /L) 14 mL,SDBS( 0. 025 mol /L) 6mL; the precursor is calcined at 300℃ for2 h. the average diameter of the product. Mn_3O_4 is 14. 52 nm, the yield is 77. 5%. Mn_3O_4 nanocrystalline shows strong effect on thermal decomposition of ammonium perchlorate, it can decrease the higher thermal decomposition temperature of AP and increase the exothermic heat significantly,and the smaller size it was,the higher catalytic activity it had.
Mn_3O_4 nanocrystalline was prepared by MnCl_2,NaOH,and H_2O_2 as the starting materials and surfactant sodium dodecyl benzene sulfonate?( SDBS) as dispersant,and it was characterized by X-raydiffraction( XRD). The catalytic properties of. Mn_3O_4 nanocrystalline on the thermal decomposition of ammonium perchlorate( AP) were investigated by differential scanning calorimetry( DSC) and thermogravimetric analysis( TG). The experimental results indicated that the optimum conditions for preparing Mn_3O_4 nanocrystalline are as follows: At room temperruture,precursor is prepared by NaOH( 0. 5mol /L) 100 mL,H_2O_2( 2. 5mol /L) 14 mL,SDBS( 0. 025 mol /L) 6mL; the precursor is calcined at 300℃ for2 h. the average diameter of the product. Mn_3O_4 is 14. 52 nm, the yield is 77. 5%. Mn_3O_4 nanocrystalline shows strong effect on thermal decomposition of ammonium perchlorate, it can decrease the higher thermal decomposition temperature of AP and increase the exothermic heat significantly,and the smaller size it was,the higher catalytic activity it had.
引文
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[14]朱俊武,陈海群,谢波,等.纳米Cu2O的制备及其对高氯酸铵热分解的催化性能[J].催化学报,2004,25(8):637-640.
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[2]黄开金.纳米材料的制备及应用[M].北京:冶金工业出版社,2009.
[3]Chen L,Horiuchi T,Mori T.Catalytic reduction of NO over a mechanical mixture of Ni Ga2O4spinel w ith manganese oxide:influence of catalyst preparation method[J].Applied Catalysis A:General,2001(209):97-105.
[4]Liu Yun-ping,Yuan Jun-jun,Lin Pei-yan,et al.Catalytic activity of nanocrystalline manganese oxides for CO oxidation[J].物理化学学报,1999,12(1):82-86.
[5]孙华银.纳米四氧化三锰催化的氧化反应及纳米铋促进的烯丁基化反应研究[D].合肥:中国科学技术大学,2011.
[6]Fang Z,Tang K B,Gao L S,et al.Facile and largescale synthesis of single-crystalline manganese oxyhydroxide/oxide nanostructures[J].M ater Res Bull,2007,42(9):1761-1768.
[7]王积森,孙金全,鲍英,等.氧化锰纳米带的合成研究[J].山东科技大学学报:自然科学版,2003,22(2):27-29.
[8]周叶青,程翔.Mn3O4纳米颗粒的制备及改性[J].应用化工,2008,37(11):1335-1337.
[9]罗元香,陆路德,刘孝恒,等.纳米Cu O的制备及对NH4Cl O4热分解的催化性能[J].无机化学学报,2002,18(12):1211-1214.
[10]马振叶,李凤生,陈爱四,等.纳米Fe2O3/高氯酸铵复合粒子的制备及其热分解性能研究[J].化学学报,2004,62(13):1252-1255.
[11]李小红,江向平,文思逸,等.不同形貌纳米α-Fe2O3粉体水热合成及其催化高氯酸铵热分解研究[J].人工晶体学报,2013(6):1132-1137.
[12]刘洪博,黄志勇,郭冰之,等.Cu/Co/Fe水滑石衍生的复合氧化物催化高氯酸铵热分解的研究[J].无机化学学报,2013(5):1077-1083.
[13]周磊,王立,俞豪杰,等.二茂铁功能化石墨烯氧化物的制备、表征及对高氯酸铵热分解的催化性能[J].材料科学与工程学报,2013(3):323-330.
[14]朱俊武,陈海群,谢波,等.纳米Cu2O的制备及其对高氯酸铵热分解的催化性能[J].催化学报,2004,25(8):637-640.
[15]罗小林,韩银凤,杨德锁.溶剂热合成Cu2O微球及其对高氯酸铵热分解的催化作用[J].物理化学学报,2012,28(2):297-302.
[16]Chen Z W,Lai J K L,Shek C H.Shape-controlled synthesis and nanostructure evolution of single-crystal M n3O4nanocrystals[J].Scripta M ater,2006(55):735-738.
[17]Fu T M,Liu F Q,Liu L.Catalytic thermal decomposition of ammonium perchlorate using manganese oxide octahedral molecular sieve(OM S)[J].Catalysis Communications,2008(10):108-112.
[18]刘建勋,李凤生,陈爱四.纳米Fe2O3的制备及其对AP热分解的催化作用[J].推进技术,2006,27(4):381-384.