精制乙基香兰素的分子蒸馏工艺研究

为解决乙基香兰素在提纯精制过程中因高温导致的热分解或聚合引起质量下降及收率降低的难题,采用分子蒸馏技术研究提纯精制乙基香兰素的低温工艺。实验中考察了压力、蒸馏温度、进料状态(温度、流速)及刮膜器的转速对乙基香兰素分离效率的影响。研究结果表明,蒸馏温度和进料速率是影响乙基香兰素纯度的2个最重要因素;适宜的工艺条件是:压力4 Pa,蒸馏温度85—90℃,进料速率120 mL/h及刮膜器转速120—140 r/m in。粗品只进行二级分子蒸馏,即可获得纯度>99%的乙基香兰素;乙基香兰素的收率提高3%—5%。     

Fatty acid esters with short‐chain alcohols in two‐phase olive pomace oils

Two‐phase decanter olive pomace (TPOP) is the by‐product of a centrifugation system, used to produce olive oil, that separates olive oil and moist pomace. The water content in these olive pomaces is about 70%, while it was 45‐50% in the olive pomace stemming from three‐phase systems (oil, water, and pomace) and 30% in the old press system. The aim of this work is focused on quantification and changes undergone during olive pomace storage in ponds of esters of fatty acids with short‐chain linear alcohols, which can be considered as a refining loss. The results indicate that oil deterioration increases very rapidly, in particular when oil is extracted from the TPOP surface. Special attention should be paid to the storage of TPOP, establishing a maximum of 2 months in all cases.     

Properties of alkyl esters base on castor oil

Castor oil is a non‐traditional raw material for the preparation of methyl and ethyl esters of higher fatty acids as alternative fuels for diesel engines. Castor oil contains ricinoleic acid (12‐hydroxy octadecene acid) with a major share of about 90%. The article presents the parameters of castor oil‐based methyl esters (COME) and ethyl esters (COEE) defined by the standard EN 14 214. The densities of COME and COEE are higher than the limit defined by the standard EN 14 214. The viscosities are more than twice as high as the limit value. The cetane numbers are lower than defined by the standard EN 14 214. For the remaining parameters, COME and COEE meet, in principle, the standard EN 14 214. The presence of the free hydroxyl group has virtually no effect on the values of such parameters as carbon residue, filterability at low temperatures and oxidation stability, for which some influence was expected. The physicochemical parameters of the castor oil esters are discussed in comparison to the analogous esters of high‐oleic sunflower oil, which contain about 80% of oleic acid. Both the methyl and ethyl esters of high‐oleic sunflower oil meet the standard EN 14 214 in all prescribed parameters.     

对叔丁基苄胺的合成研究

摘要选择Delepine反应法的路线合成对叔丁基苄胺，并对反应投料比、反应温度及酸化后的反应时间进行了优化试验，得到了较好的反应条件：反应温度为40℃，对叔丁基苄氯与乌洛托品投料比为1：1；加入酸和醇后的保温时间为2h，从而使反应收率稳定在90％以上，含量达到95％。     

(Z)-4-氯-2-羟亚胺基乙酰乙酸乙酯的合成

采用4-氯乙酰乙酸乙酯为原料,对(Z)-4-氯-2-羟亚胺基乙酰乙酸乙酯的合成条件进行了研究,确定了优化条件:反应温度5℃、反应时间4h、亚硝酸乙酯气体与4-氯乙酰乙酯的摩尔比n(ONOC2H5)∶n(ClCH2COCH2CO2C2H5)=1.4∶1。优化条件下产物收率约96%。     

Addition of ferulic acid,ethyl ferulate,and feruloylated monoacyl- and diacylglycerols to salad oils and frying oils

To determine antioxidative effects of ferulic acid and esterified ferulic acids, these compounds were added to soybean oils (SBO), which were evaluated for oxidative stability and frying stability. Additives included feruloylated MAG and DAG (FMG/FDG), ferulic acid, ethyl ferulate, and TBHQ. After frying tests with potato chips, oils were analyzed for retention of additives and polar compounds. Chips were evaluated for hexanal and rancid odor. After 15 h frying, 71% of FMG/FDG was retained, whereas 55% of ethyl ferulate was retained. TBHQ and ferulic acid levels were 6% and <1%, respectively. Frying oils with ethyl ferulate or TBHQ produced significantly less polar compounds than SBO with no additives. Chips fried in SBO with TBHQ or ferulic acid had significantly lower amounts of hexanal and significantly less rancid odor after 8 d at 60°C than other samples. Oils were also aged at 60°C, and stability was analyzed by PV, hexanal, and rancid odor. Oils with TBHQ or FMG/FDG had significantly less peroxides and hexanal, and a lower rancid odor intensity than the control. FMG/FDG inhibited deterioration at 60°C, whereas ethyl ferulate inhibited the formation of polar compounds in frying oil. Ferulic acid acted as an antioxidant in aged fried food. TBHQ inhibited oil degradation at both temperatures. Presented at the 94th AOCS Meeting & Expo, Kansas City, MO, May 4–7, 2003.     

锝萃取型发生器萃取锝初探

锝萃取型发生器技术是采用溶剂萃取的方法生产^99Tc^m。对锝萃取工艺条件进行了初步研究。由于锝与铼有相似的化学性质,实验中研究了在碱性体系中甲乙酮对铼的萃取行为,考察了萃取剂用量、碱液浓度、铼的浓度及水相中铝浓度对萃取铼的影响,在此基础上进行了^99Tc^m的示踪实验,实验结果表明：甲乙酮对^99Tc^m萃取率达99％。     

一锅法合成2-溴甲基苯并咪唑和3，4-二氢-1H-喹喔啉-2-酮

以邻苯二胺和溴代乙酸乙酯为原料一步合成了2-溴甲基苯并咪唑和3,4-二氢-1H-喹喔啉-2-酮．研究结果表明,这两种物质的生成具有伴生性．     

Study on volume ratio and plasticizer screening of free coating membranes composed of ethyl cellulose and chitosan

The aim of this study was to optimize the formula of free blended coating membrane of ethyl cellulose (EC) and chitosan (CS), including their suitable ratio range and the best plasticizer used. The dry films were produced by a casting/solvent evaporation method, with different volume ratio of EC and CS solution plasticized by various plasticizers, respectively. The wet films were prepared by immersing dry films in pH 6.8 phosphate buffer saline (PBS) for 24 h. The promising ratio range of EC/CS was below 20/5 or 20/6 with various plasticizer, which was determined by comparing the viscosity of the blended solutions and the morphology of the blended films. The efficiency of plasticization was evaluated by measuring glass transition temperature (T_g). All the testing plasticizers have good compatibility with EC or CS and dibutyl phthalate (DBP) have the strongest efficiency inducing the lowest T_g (39.9°C) of the film. Mechanical properties were evaluated by the ratio of tensile strength (T) to elastic modulus (E). In the wet state, the films with DBP had the highest T/E value (1.2). The results of leaching of plasticizers also verified that DBP was the most stable plasticizer in the films. The release rates of tetramethylpyrazine phosphate (TMPP) through the pellets coated with the blended films of EC/CS (20 : 6 v/v) plasticized by various plasticizers showed that the more water‐soluble the plasticizer was, the more quickly TMPP dissolved from the coated pellets, which further indicated that the water‐insoluble plasticizers (such as DBP) could be more applicable to keep the sustained or controlled release property of the blended films in wet state. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1932–1939, 2006     

油酸二聚甘油酯的合成及其柔软保湿纸的测试

以油酸缩水甘油酯和甘油为原料，在固体酸催化剂（活性炭负载硫酸）作用下，通过开环反应制得油酸二聚甘油酯。通过FTIR和1HNMR对产物结构进行表征，并将其用作柔软保湿剂涂覆到面巾纸上对纸张的柔软度、保湿性、抗张强度等性能进行测试。结果表明：油酸二聚甘油酯具有优异的柔软保湿性能，在油酸二聚甘油酯添加量为甘油水溶液质量的0.25%时，面巾纸的柔软度（49 mN）优于市面上有机硅柔软剂改性的面巾纸柔软度（68 mN），这是由于大分子柔软剂能够对纤维表面的缺陷进行修复，从而使纤维表面平整度的提升。且在温度为30 ℃，湿度为60%时，油酸二聚甘油酯型柔软保湿剂涂覆后的面巾纸的保水率（98.2%）也略高于有机硅柔软剂涂覆后的面巾纸的保水率（96.5%）。