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1.
纳米Co3O4的制备及其对高氯酸铵热分解的催化性能   总被引:5,自引:0,他引:5  
 选用CoCl2·6H2O分别与NaOH, H2C2O4·2H2O, Na2CO3·10H2O及Na2C2O4组成四个反应体系,通过室温固相反应制备了不同平均粒径的纳米Co3O4, 并用X射线衍射和透射电镜对Co3O4的物相、形貌和粒径大小进行了表征. 结果表明, Co3O4的平均粒径分别为23, 30, 35和150 nm, 大小均匀,分散性好. 还用差热分析法考察了纳米Co3O4对高氯酸铵热分解的催化性能,并与微米Co3O4进行了比较. 结果表明,纳米Co3O4可使高氯酸铵的低温放热峰消失,高温放热峰温度降至323.5 ℃, 降低了128.5 ℃, 表观分解热增加了750 J/g, 达 1265 J/g, 纳米Co3O4对高氯酸铵热分解的催化性能明显好于微米Co3O4.  相似文献   

2.
草酸钴原位催化高氯酸铵热分解的DSC/TG-MS研究   总被引:5,自引:0,他引:5  
采用差示扫描量热/热分析-质谱(DSC/TG-MS)联用技术研究了草酸钴对高氯酸铵的原位催化. 结果表明,草酸钴原位分解生成的钴氧化物对高氯酸铵有较强的催化作用,添加2%的草酸钴使高氯酸铵的分解温度降低104 ℃, 分解放热量从655 J/g增大到 1 469 J/g. 分解的气相产物主要有H2O, NH3,O2,HCl,Cl2,NO,N2O和NO2. 由于氧在新生态的纳米钴氧化物表面形成过氧化活性离子(O-2), 使氨氧化在钴氧化物的过氧化表面活性中心进行,加速了高氯酸铵的热分解,使其表观放热量大幅度增加.  相似文献   

3.
采用化学液相沉淀法制备Y2O3纳米粒子/碳纳米管复合体(Y2O3/CNTC),利用扫描电镜(SEM)和X 射线光电子能谱(XPS)对其结构和成分进行了表征. 结果表明, Y2O3纳米粒子能负载在碳纳米管上,且负载效果较好. 采用差热分析研究了Y2O3/CNTC 对高氯酸铵热分解的催化性能, 结果表明, Y2O3 /CNTC 可显著降低高氯酸铵(AP)的高温分解峰温,表现出对AP 高温分解良好的催化性能. 相同量的Y2O3/CNTC 和纯Y2O3纳米粒子进行对比, Y2O3 /CNTC表现出更强的催化性能.当Y2O3/CNTC的质量分数为4%时,使AP的高温分解峰温提前131.14C[deg].  相似文献   

4.
以硝酸镧和硝酸钴为原料,通过硬脂酸法制备了纳米LaCoO3。采用红外光谱、X射线衍射、透射电镜等测试手段对产物进行了表征,并用热分析法考察了不同含量的纳米LaCoO3对高氯酸铵热分解的催化作用。结果表明,在600℃下可获得结晶良好的钙钛矿型纳米LaCoO3,粒径约40-60 nm。纳米LaCoO3能强烈催化高氯酸铵的热分解,催化作用随着LaCoO3含量的增加而增强。添加5%的纳米LaCoO3可使高氯酸铵的高温分解温度下降116℃,分解放热量也由2%时的1390 J·g^-1增至1600 J·g^-1。  相似文献   

5.
以Cu/Co/Fe水滑石(Cu/Co/Fe-LDHs)为前驱体经过焙烧制备了Cu/Co/Fe复合氧化物(Cu/Co/Fe-MOs)。利用DTA和TG-MS研究了Cu/Co/Fe-MOs作为新型催化剂对高氯酸铵热分解的催化性能。结果表明,Cu/Co/Fe-MOs呈现为CuFe2O4和(CoFe2)O4晶相,具有70~110 m2.g-1的比表面积。晶粒大小均匀,尺寸在20~30 nm。添加4wt%的400℃焙烧得到的Cu/Co/Fe-MOs催化剂使高氯酸铵热分解反应的温度降低了139℃。Cu/Co/Fe-MOs是通过吸附在金属氧化物表面的超氧离子(O2-)来加速高氯酸铵热分解的。  相似文献   

6.
以聚乙烯吡咯烷酮(PVP)为添加剂,利用溶剂热法合成了Cu2O微球.考察了PVP用量以及反应温度对产物形貌的影响,并在反应时间为2.5与4.5h时分别合成了直径为100-200nm和1μm的Cu2O微球.同时,利用差热分析(DTA)技术考察了不同直径的Cu2O微球对高氯酸铵(AP)热分解的催化效果,结果表明:添加2%(w)的直径为100-200nm和1μm的Cu2O微球使得AP的高温分解温度分别降低了116和118°C,AP在低温阶段的分解量也明显提高.  相似文献   

7.
纳米Fe2O3/高氯酸铵复合粒子的制备及其热分解性能研究   总被引:8,自引:1,他引:7  
马振叶  李凤生  陈爱四  白华萍 《化学学报》2004,62(13):1252-1255,J004
用溶剂-非溶剂法制备了纳米Fe2O3/高氯酸铵(AP)复合粒子,并用TEM,SEM,XRD和ICP对其进行了表征.为了研究纳米复合粒子中纳米Fe2O3对AP热分解的催化性能,将相同比例的微米Fe2O3和纳米Fe2O3与AP分别简单混合后作对比,并用DTA对三种样品进行了热分析.结果表明,三种样品中的Fe2O3粒子都能催化AP的热分解;但纳米Fe2O3粒子的催化性能优于微米Fe2O3粒子,纳米Fe2O3/AP复合粒子中纳米Fe2O3对AP的催化性能优于纳米Fe2O3与AP简单混合物.与纳米Fe2O3与AP简单混合的样品相比,纳米复合粒子中的AP高温分解峰温降低20.1℃,低温分解峰几乎消失,表观分解热由850.2J/g提高到1080.8J/g.证明纳米Fe2O3与AP的复合处理能显著提高纳米Fe2O3对AP热分解的催化性能.并用不同样品中AP热分解的动力学参数对所得结果进行了理论分析.  相似文献   

8.
以CuSO4.5H2O和NaOH为原料,采用沉淀法制备得到Cu(OH)2纤维,再进行Cu(OH)2的分解反应.考察了在不同实验条件下温度对Cu(OH)2热分解过程的影响.结果表明:在反应温度20℃,反应终点pH值为12,搅拌速度为1 200 r.min-1,NaOH溶液的滴加速度为50 mL.min-1的反应条件下,得到的样品为纳米Cu(OH)2纤维,其直径为10~30 nm、长度为1~6μm;在固相纳米Cu(OH)2热分解制备CuO过程中CuO粒径随温度的升高而增大,在温度不超过200℃时CuO的粒径约为20 nm左右;在液相中先沉淀后升温时,产物的形貌为球形,CuO粒径随温度的升高而增大,低于80℃可得到纳米级的CuO.  相似文献   

9.
采用超声法和微波水热法,制备了棒状、球状、梭形和杨桃状纳米CuO粉体。以X-射线粉末衍射仪(XRD)、透射电镜(TEM)手段对各种产物进行了表征。用热分析法考察了不同形貌的纳米CuO对高氯酸铵(AP)分解的催化作用。结果表明,四种形貌的纳米CuO均可强烈催化AP的热分解,而棒状和球状纳米CuO的催化活性更高。与纯高氯酸铵相比,加入棒状纳米CuO后AP的高温分解温度降低了124.4 ℃,加入球形纳米CuO催化剂后高温分解温度降低了122 ℃,且低温分解峰消失。  相似文献   

10.
郭琦  缪建军  耿珺  朱俊杰 《应用化学》2010,27(12):1438-1443
在二乙二醇溶剂体系中利用微波介电加热分解醋酸铜前体,进一步还原得到Cu2O和Cu纳米粒子以及Cu/Cu2O核壳结构。采用X射线衍射、透射电子显微镜、扫描电子显微镜和紫外吸收光谱测试技术对产物的形貌、结构和组成进行了研究,结果表明,得到的Cu/Cu2O核壳结构直径为500nm左右。对比实验研究了不同聚合度乙二醇系列溶剂、反应时间以及表面活性剂或配位剂对产物形貌、组成的影响,表明低聚合度乙二醇和长的反应时间有利于醋酸铜还原形成铜。  相似文献   

11.
The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.  相似文献   

12.
非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。  相似文献   

13.
翟宗玺  刘树深  夏树屏 《化学学报》1990,48(10):946-950
用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。  相似文献   

14.
Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.  相似文献   

15.

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

  相似文献   

16.
Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.  相似文献   

17.
Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, Mo, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.  相似文献   

18.
In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.  相似文献   

19.
20.
The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe2O3. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

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