二苯基硫脲—甲基异丁酮泡沫塑料富集——XRF测定痕量金

报道了在１０％王水介质中，有Ｂｒ２存在时用二苯基硫脲—甲基异丁酮泡沫塑料富集、Ｘ射线荧光测定痕量金的分析方法。     

微波与传统水热法合成丙酸锌

采用微波水热法和传统水热法以氧化锌和丙酸为原料、去离子水为溶剂成功合成了丙酸锌(C6H10O4Zn)。对比考察了两种合成方法中单因素(反应温度、反应时间、丙酸/氧化锌摩尔比、去离子水量)对丙酸锌产率的影响;利用EDTA络合滴定、元素分析仪(EA)、红外光谱仪(FTIR)和热重分析仪(TG)分析了丙酸锌的组成与结构。结果表明,在最优化反应条件下,微波水热法和传统水热法合成丙酸锌的产率分别为94.06%和87.34%;与传统水热法相比,微波水热法对丙酸锌制备过程具有强化作用。采用两种不同方法所合成的样品都具有典型的丙酸锌结构,组成略有差异,微波条件下的丙酸锌含更多结晶水,热稳定性更好。     

硫酸高铈改性离子交换树脂催化合成丁酸异丁酯的研究

采用硫酸高铈与阳离子交换树脂反应制备的改性离子交换树脂催化合成丁酸异丁酯。考察了催化剂用量、醇酸物质的量比、反应时间、带水剂种类及催化剂重复使用性等因素对收率的影响。结果表明该催化剂与反应体系形成非均相物系,具有易分离回收,催化活性高,反应时间短,出水速率快,合成工艺流程简单,操作方便,不易腐蚀设备,废液排放量少,不需加带水剂即可获得较为理想的收率等优势,基本革除了浓硫酸为酯化催化剂存在的设备腐蚀严重、后处理工艺复杂、废液排放量多等弊端。硫酸高铈改性离子交换树脂是合成丁酸异丁酯的高效、经济且环境友好的酯化催化剂,具有一定的工业化应用前景。适宜反应条件为:正丁酸0.15mol,醇酸物质的量比1.3,催化剂2.0g,反应时间40min,收率85.7%。     

乳液法合成氯乙烯/乙烯基异丁醚共聚树脂

介绍了10L聚合釜乳液法氯乙烯/乙烯基异丁醚共聚树脂研制开发状况。讨论了pH值缓冲剂、聚合温度、引发体系、乳化剂等对合成氯醚树脂的影响规律。     

钨硅酸催化合成丁酸异丁酯的研究

以钨硅酸为催化剂,通过丁酸和异丁醇反应合成了丁酸异丁酯,探讨醇酸物质的量比、催化剂用量及反应时间对酯化率的影响。实验结果表明:钨硅酸具有良好的催化活性,在醇酸物质的量比为1.3∶1、催化剂用量为0.5g/0.15mol酸、反应温度120~137℃、反应时间1h,酯化率可达99.1%。     

Measurement and correlation of the solubility of two steroid drugs in supercritical carbon dioxide using semi empirical models

The solubilities of desoxycorticosterone acetate (DA) and clobetasole propionate (CP) in supercritical carbon dioxide (SC-CO₂) were measured at temperature ranging from (308 to 348) K and pressures from (12.2 to 35.5) MPa using a static method. The mole fraction solubilities ranged from 10⁻⁷ to 13.93 × 10⁻⁵. The crossover region was observed for DA and CP at 24.3 and 25.3 MPa, respectively. Solubility data were correlated using four semi-empirical density-based models (Chrastil, Bartle, Kumar, Johnston (K–J) and Mendez-Santiago and Teja (M–T) models). The average absolute relative deviations (AARD%) ranged from 9.3 to 13.6; 8.9 to 11.9; 6.5 to 10.3 and from 10.4 to 13.4 for Chrastil, Bartle, K–J and M–T models, respectively. A comparison among the four models revealed that the K–J model gave much better correlation of the solubilities in comparison with other models. Using the correlation results, the heat of drug–CO₂ solvation and that of drug vaporization was separately approximated in the range of −24.2 to −24.5 and 63.8 to 64.8 kJ mol⁻¹. The correlation results showed good agreement with the experimental data.     

Methane oxidation on alumina supported palladium catalysts: Effect of Pd precursor and solvent

Palladium precursors and solvents were studied for their effects on the activities of alumina-based palladium catalysts in methane combustion and the resistance of the catalysts to thermal aging. The properties of the catalysts were compared with those of a commercial reference. The palladium precursors were Pd(propionate)₂, Pd(acetate)₂ and Pd(acetyl acetonate)₂ and the solvents were acetone, acetic acid, propionic acid and toluene. Catalysts were prepared by the wet impregnation method.Catalysts were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy (EDS). The surface areas were measured by Brunauer–Emmett–Teller method (BET). Acidity of the alumina support was measured by NH₃ desorption. Activities of the catalysts in methane oxidation were screened under lean burn conditions.In methane oxidation with fresh catalyst, the best performance was obtained with a combination of Pd(acetate)₂ and acetic or propionic acid. The light-off temperatures of the fresh catalysts (562 K and 557 K, respectively) were slightly lower than the light-off temperature (567 K) of the commercial reference. Differences between the light-off temperatures of the aged and fresh catalysts were least when the catalysts were prepared with Pd(acetyl acetonate)₂ as Pd precursor and in acetic or propionic acid as solvent: +12 K and +18 K, respectively. The corresponding value for the reference was +64 K. For several of the fresh catalysts, conversion in methane oxidation at 623 K was over 90%. A comparison of methane combustion and NH₃ desorption results indicated that acidity of the support material affects catalysts activity.     

食品级丙酸锌的合成工艺研究

以丙酸钙和硫酸锌为原料，经分解反应合成了一种新型食品添加剂－丙酸锌，此反应的优化条件是：n(丙酸锌）:n(硫酸锌）＝1.16:1，c(丙酸钙）＝1.075mol/L,c（硫酸锌）＝1.239mol/L，反应温度为80℃，反应时间为40min，丙酸锌产率可达93.6%，其各项技术指标经检测符合同类产品食品级标准要求。     

饮料酒中甲醇与杂醇油的气相色谱法分析

为了提高酒中甲醇、杂醇油测定的精密度和准确度,节省分析时间和分析成本。本实验探索研究采用丙酸乙酯作为用气相色谱法的内标物,测定饮料酒中的甲醇和杂醇油（异丁醇、异戊醇）含量的方法。采用GDX-102不锈钢填充柱进行分离,氢火焰离子化检测器检测,利用保留时间定性,并以丙酸乙酯作内标定量,并顺带测定了其中的乙酸乙酯、正丙醇和正丁醇的含量。得到了令人满意的结果：方法的准确度高,7种组分的加标回收率在90．1％～108．8％之间;方法的重现性精密度即相对标准偏差在0．00％～5．37％之间,符合国标规定的气相色谱的测定误差不大于10％的要求。     

丙酮一步法合成甲基异丁基酮催化剂的失活机理

为研究丙酮一步法合成甲基异丁基酮Pd/Al2O3催化剂的失活机理,采用BET,XRD,SEM,O2-TPO等方法,对反应前后的催化剂进行了表征。表征结果表明,反应前后催化剂中的Pd含量没有明显变化,而反应后的催化剂表面织构变化较大,反应后的催化剂孔体积减小、平均孔径增大,Al2O3载体形态由γ型转化为羟基氧化铝的形态;同时,反应后的催化剂表面存在一定的高沸物。因此,催化剂加氢能力降低的主要原因是载体Al2O3形态的变化和催化剂表面包覆的高沸物,造成加氢活性中心减少。