共查询到20条相似文献,搜索用时 62 毫秒
1.
建立了动态和静态接口装置,使其能在线联用超临界色谱确定蒽在超临界二氧化碳中的溶解度及溶解平衡过程。静态接口由2个高压阀组成,动态接口由1个高压阀和1个齿轮泵组成。采用静态法测定蒽在超临界二氧化碳中的溶解度,以考察温度和压力对溶解度的影响。实验结果表明,在40~60℃和10~27.5MPa条件下,自行研制的在线超临界色谱联用体系具有较高的稳定性和较好的重现性,溶解度的相对标准偏差(RSD)为0.4%~2.4%,准确性为95.0%~97.7%。采用Méndez-Santiago Teja(MST)模型公式对实验数值关联计算,确定了蒽的溶解度与二氧化碳密度的准线性函数变化关系,计算数值与实验结果之间的相对平均绝对值偏差(AARD)为3.23和14.68。搭建的接口装置亦能够完成超临界流体技术与常规光谱、质谱分析仪器的在线联用分析,在药物合成与分析、过程分析技术(PAT)等领域具有较好的应用潜力。 相似文献
2.
用色谱保留值法测定了单质碘和单斜硫在不同温度及压力下在超临界二氧化碳中的溶解度,并用超临界平衡饱和萃取法验证了测定值,结果满意。 相似文献
3.
探索了聚乙二醇双丙烯酸酯在超临界二氧化碳中发生光聚合反应制备聚合物颗粒的过程.方法为向充满超临界二氧化碳的高压反应釜中,同时喷射二氧化碳与聚乙二醇双丙烯酸酯及光引发剂的溶液,溶液与二氧化碳形成均匀的喷雾并进一步通过反溶剂作用与超临界二氧化碳形成分散体系,当同步进行紫外光照射时,单体可以在超临界二氧化碳中发生光聚合.结果证明此方法是可行的,得到了聚合物微颗粒.研究了不同溶剂及反应原料用量对产物粒径分布的影响.采用不同溶剂,将改变反应原料及产物在超临界二氧化碳中的溶解度,进而改变产物的粒径分布;反应原料用量增加,其在超临界二氧化碳中的溶解度减小,导致产物粒径分布较宽。 相似文献
4.
5.
有关分散染料与超临界CO2二元体系的相平衡数据(溶解度)实验测定及模型关联,对超临界流体染色工艺基础研究及工业化至关重要。本文建立了高压溶解度测试实验装置,在温度353~393K、压力15~30MPa条件下,对分散红60在超临界CO2中的溶解度进行了测定。并利用zcan经验公式对实验结果进行关联,关联结果和实验结果吻合较好,最大误差为9.3%。结果表明:体系的压力、温度和混合物密度是影响分散染料在超临界CO2中溶解度的重要因素;可利用zcan经验公式对染料等固体物质在超临界CO2中的溶解度进行关联计算。 相似文献
6.
由于超临界二氧化碳(SCCO2)具有稳定、安全、不燃、清洁无毒、粘度小、扩散快、可压缩的特殊性质,所以使得超临界二氧化碳非常适合作为催化反应的绿色溶剂.除此之外,多种气体在超临界二氧化碳中的溶解度很高,这对于那些受传质阻碍和易引起安全隐患的气相反应来讲,使用SCCO2作为替代的反应溶剂具有重要的价值。值得指出的是:如果选择超临界二氧化碳作为氧化反应的溶剂,其自身不会发生反应而产生副产物,从而容易得到清洁的产物。本文主要讨论了超临界二氧化碳作为反应介质对醇、烯烃和烷烃等选择氧化反应的影响,通过与传统溶剂比较可以看出超临界二氧化碳作为氧化反应溶剂的优势,对近几年来以分子氧为氧化剂,以超临界二氧化碳为介质的催化选择氧化的反应体系作了综述,并对未来的发展提出了展望。 相似文献
7.
8.
以超高分子量聚乙烯作为原料, 在超临界二氧化碳中通过热处理成功制备了聚合物微米球. 微球尺寸符合高斯分布, 并可以控制在较窄范围内, 微球表面多孔且内部中空. 微球的形成是恒温过程和超临界二氧化碳双重作用的结果. 降温过程导致聚合物溶解度降低, 超高分子量聚乙烯分子链析出结晶而形成微球, 内部包裹了少量二氧化碳; 温度进一步降低导致微球内外压力不平衡, 二氧化碳从空心球内部释放形成表面孔洞. 恒温结晶过程除了促使微球结晶度进一步提高外, 还可以使亚稳晶型单斜晶转化为稳定的正交晶. 相似文献
9.
10.
11.
Supercritical fluid extraction (SFE) provides for the first time a viable option to conventional and widely used Soxhlet extraction. The ability to change the solvating power of a single supercritical fluid by changing its density is an exceedingly attractive feature. An environmentally safe alternative such as supercritical carbon dioxide to organochlorine solvents which are widely used today in many government and industrial analytical laboratories for sample preparation is desirable. SFE may also constitute a viable alternative to other popular sample preparation techniques such as liquid-liquid extraction, solid phase extraction and purge/trap. Much research, however, must be done in order to understand, optimize and apply this technology. For example, (a) automation of extraction, (b) matrix effects, (c) new fluids/modifiers/additives, (d) trapping efficiency, (e) recovery of extracted analytes, and (f) extraction kinetics are some areas which need a greater understanding. This review is concerned with many of these topics as they relate to trace organic analysis wherein SFE is the primary sample preparation technique. 相似文献
12.
13.
14.
Dirk Brll Claudia Kaul Alexander Krmer Petra Krammer Thomas Richter Matthias Jung Herbert Vogel Peter Zehner 《Angewandte Chemie (International ed. in English)》1999,38(20):2998-3014
Water is a special liquid —and not only under “normal” conditions. Water in the supercritical state (shaded area in the phase diagram) is distinguished by special properties which are wholly at variance with those of normal water. So far these have usually been exploited for the purification of waste water, for example for the complete oxidation of poorly degradable substances. But what is the potential of supercritical water for synthesis? Answers are provided here on the basis of thermodynamic and kinetic studies as well as with reference to measurements of corrosion. 相似文献
15.
Adsorption isotherms for supercritical fluids are calculated using lattice theory. Results are compared with experimental data for methane on graphon and for carbon dioxide on coal. It is shown that the model reflects the peculiar features in adsorption isotherms of supercritical fluids (in particular, a maximum in the adsorption with increasing pressure). The analysis shows that there is two layer adsorption over a wide range of densities. 相似文献
16.
JM Bernal P Lozano E García-Verdugo MI Burguete G Sánchez-Gómez G López-López M Pucheault M Vaultier SV Luis 《Molecules (Basel, Switzerland)》2012,17(7):8696-8719
The synthesis of biodiesel fuel from lipids (vegetable oils and animal fats) has gained in importance as a possible source of renewable non-fossil energy in an attempt to reduce our dependence on petroleum-based fuels. The catalytic processes commonly used for the production of biodiesel fuel present a series of limitations and drawbacks, among them the high energy consumption required for complex purification operations and undesirable side reactions. Supercritical fluid (SCF) technologies offer an interesting alternative to conventional processes for preparing biodiesel. This review highlights the advances, advantages, drawbacks and new tendencies involved in the use of supercritical fluids (SCFs) for biodiesel synthesis. 相似文献
17.
The growth of octadecyltrimethylammonium bromide (C(18)TAB) monolayers on mica was investigated using atomic force microscopy and infrared spectroscopy. A critical temperature was identified below which the monolayer formed via an "islanding" mechanism, that is, nucleation and growth of densely packed two-dimensional (2D) islands within a matrix of a disordered dilute phase. However, above the critical temperature, there was no coexistence of 2D phases during film formation. Instead, the monolayer gradually became better ordered, remaining laterally homogeneous throughout. We show that this corresponds to a critical point in a 2D phase diagram of the monolayer. Additional evidence is provided by the in situ observation of 2D phase separation upon cooling an incomplete monolayer from the one-phase to the two-phase region. The lack of coexisting domains (and domain boundaries) during growth above the critical point provides a possible route for the preparation of essentially defect-free monolayers. 相似文献
18.
19.
20.
E. Klesper 《Angewandte Chemie (International ed. in English)》1978,17(10):738-746
Chromatography with supercritical fluids unites the features of both gas chromatography and liquid chromatography, yet retains special characteristics of its own. The diffusion coefficient and particularly the viscosity of fluid phases may approach values for low-pressure gases, while the solvent power may be similar to that of liquids. However, with supercritical fluids it is possible to control chromatographic separations very effectively by pressure programming, since the solubility increases with increasing density. Temperature programming, on the other hand, can have the opposite effect to that in gas- or liquid-chromatography since the density decreases with increasing temperature at a given pressure. Supercritical fluid chromatography is primarily of interest for the separation of higher molecular weight compounds. The efficiency of this method of separation is demonstrated on several homologous series. Thus, a styrene oligomer with nominal Mw=2200 can be resolved by a pressure and temperature program into 40 species. 相似文献