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。     

Continuous liquid-phase valorization of bio-ethanol towards bio-butanol over metal modified alumina

Commercial mixed-phase aluminum oxide was used as a heterogeneous catalyst support, providing slightly basic properties which are well-suited for the condensation of bio-ethanol to C₄ hydrocarbons, such as 1-butanol. Different metals (Cu, Ni and Co), at various metal loadings were deposited on the support. Consequently, the catalytic reactions were carried out in a continuous laboratory-scale fixed bed reactor operated at 240 °C and 70 bar. The catalysts were characterized by means of XRD, TEM, FT-IR, XPS and ICP-OES. Different metals were found to give entirely different product distributions. With the best catalysts, the selectivities towards 1-butanol close to 70% were reached, while the ethanol conversion typically varied between 10 and 30% – strongly depending on the metal applied. It was observed that low loading of copper and high loading of nickel were responsible for the formation of 1-butanol, whereas cobalt and high loading of copper resulted in the production of ethyl acetate. The reaction was found to be extremely sensitive to catalyst preparation conditions and procedures such as metal loading, calcination/reduction temperature and, thereby, to the formation of corresponding crystallite structure.     

正己烷和乙酸乙酯间歇共沸精馏分离共沸剂的研究

正己烷和乙酸乙酯形成最低共沸物,采用间歇共沸精馏方法分离回收时,共沸剂的选择和用量直接影响实验效果。研究了正己烷-乙酸乙酯共沸物系间歇共沸精馏法分离适宜的共沸剂,并从理论上和实验中考察了共沸剂与原料适宜的配比。实验结果表明,丙酮为合适的共沸剂,当丙酮和正己烷的质量比为1.15时,正己烷和乙酸乙酯的收率最高,分别达75.15%和73.89%。通过实验绘制了正己烷-乙酸乙酯-丙酮三元物系的剩余曲线,确定了正己烷-乙酸乙酯共沸物系分离步骤:共沸精馏塔中馏出丙酮和正己烷的共沸物和高纯度的乙酸乙酯;萃取塔中用水萃取丙酮和正己烷的混合物得到较纯的正己烷;萃取后的丙酮水溶液由共沸剂精馏回收塔回收丙酮。     

溶解乙炔气瓶安全运输要点

介绍了乙炔的特性，并根据其特性提出运输溶解乙炔气瓶时，如何保护汽车驾驶员、押运员、装卸人员以及沿途群众和建筑物等安全运输要点。     

国内外丙酮生产现状与市场分析

2003年全球丙酮的总产能为560万t/a,按地区分布为北美33%,西欧29%,东欧14%,日本9%,其他15%。丙酮主要用做溶剂,其次是生产丙酮氰醇、MMA和双酚A。2004年我国丙酮的产能为30.1万t/a,主要生产厂家有上海高桥石化、燕山石化、吉林化学工业公司和哈尔滨华宇股份有限公司。双酚A的消费需求将拉动丙酮的需求,预计2008年我国丙酮的产能将达到61.2万t/a。     

Optimisation of tripalmitin‐rich fractionation from palm stearin by response surface methodology

BACKGROUND: Solvent fractionation is effective in improving separation at low temperature, resulting in higher yield and purity of the final product. Tripalmitin (PPP) is an important substrate for the synthesis of human milk fat substitute (HMFS). In this study a fraction rich in PPP was separated from palm stearin by solvent fractionation. RESULTS: The PPP‐rich fraction was concentrated from palm stearin by acetone fractionation. Response surface methodology (RSM) was employed to optimise PPP purity (Y₁, %) and PPP content (Y₂, g kg^?1 palm stearin) with the independent variables fractionation temperature (X₁, 25, 30 and 35 °C) and weight ratio of palm stearin to acetone (X₂, 1:3, 1:6 and 1:9). The predictive models for PPP purity and PPP content of the solid fraction were adequate and reproducible, with no significant lack of fit and satisfactory levels of R². PPP purity showed a positive correlation with temperature and acetone ratio, whereas PPP content exhibited a negative correlation. The optimised fractionation condition for a targeted PPP‐rich fraction with > 92% PPP purity and > 225 g kg^?1 PPP content from palm stearin was predicted. CONCLUSION: The RSM model for optimising PPP purity and PPP content in the PPP‐rich fraction from palm stearin by acetone fractionation was valid. The scaled‐up PPP‐rich fraction obtained can be used as a substrate for the synthesis of 1,3‐dioleoyl‐2‐palmitoylglycerol, which is a main component of HMFS in infant formulas. Copyright © 2010 Society of Chemical Industry     

PTA装置脱水塔回流液成分分析

建立了PTA装置脱水塔回流液成分分析的气相色谱法,选用CP-si18CB毛细管色谱柱和程序升温技术,又使沸点、极性接近的复杂组分得到很好地分离,并解决了醋酸严重拖尾的问题。另外,采用内标法对回流液中每个组分进行含量测定,对工艺操作有一定指导作用。     

丙酮-丁醇精馏工艺中丁醇塔的优化模拟

针对发酵法的丙酮-丁醇精馏工艺中能耗较高的问题,提出一个优化方案:在醪塔增加一个侧线出料,醪塔的侧线与塔顶出料分别从不同位置进入丁醇塔,并增加丁醇塔的塔高,同时将丁醇塔内的分相罐移至塔外。采用PRO/Ⅱ化工流程模拟软件对优化后的丁醇塔进行模拟计算,考察了理论塔板数、进料位置、回流比对分离性能的影响。优化的丁醇塔为40块理论塔板,两股进料位置分别为第8块和第14块理论塔板,回流比为4。在此条件下,丁醇塔塔顶馏出物中水的质量分数由8.56%降为2.18%,丁醇的质量分数由2.71%降为微量,蒸汽消耗量与原丁醇塔相比降低了52.6%。工业试运行结果与优化结果吻合良好。     

MgFe2O4纳米复合氧化物的制备和气敏性能

用反滴定化学共沉淀法制备了纳米尺寸尖晶石型的复合金属氧化物MgFe2O4粉体.用X射线粉末衍射分析、透射电镜等手段研究了其结构特性.MgFe2O4粉体颗粒均匀,700℃煅烧1 h粉体平均粒径约为20 nm.研究表明煅烧温度对材料的结构及性能有较大的影响.以MgFe2O4纳米粉体为原料制备了旁热式气敏元件,测试了元件的敏感特性和响应恢复特性.结果显示,MgFe2O4是一种良好的n型半导体气敏材料,700℃煅烧1 h所得纳米粉体制作的元件在300℃工作温度时对CH3COCH3有较高灵敏度和良好的选择性,对体积分数为1 000×10-6的CH3COCH3的灵敏度可达36.87.并对气敏机理给予了解释.     

花状ZnO纳米棒的合成及丙酮敏感特性的研究

利用水热法合成花状的ZnO纳米棒,并对其进行X射线衍射（X-ray diffraction, XRD)与扫描电子显微镜（scanning electron microscope, SEM) 表征.以该ZnO为敏感材料制成了旁热式结构气体传感器,测试了样品在不同温度下对丙酮气体的灵敏度.结果表明样品在290℃下对于丙酮气体具有高的灵敏度、快的响应恢复速度等特点.测试了传感器对于常见干扰气体的灵敏度,表明器件具有良好的选择性.