均相无溶剂法合成蔗糖酯

以生物表面活性剂为催化剂,用均相无溶剂法在不同条件下合成了蔗糖酯。小试的转化率达到５０％￣５５％,产品质量符合ＧＢ８２７２０８７标准,使蔗糖酯的合成达到了先进水平。     

蔗糖酯表面活性剂化学合成工艺研究进展

蔗糖酯表面活性剂作为一种广受关注的生物基表面活性剂,大量应用于食品、医药和化妆品等领域。当前,蔗糖酯的合成主要采用直接酯化、酰氯酯化和酯交换法进行,其中酯交换法是最常用的方法,然而蔗糖与甲酯相容性差导致其存在蔗糖焦化结块、甲酯水解和皂化等副反应,严重影响反应效率和产品性能。基于此,该文对溶剂法、微乳化法和无溶剂法等蔗糖酯合成工艺进行了介绍,随后,着重介绍了相转移催化剂、固体碱催化剂、离子液体等新型催化技术和物理界面强化技术在蔗糖酯合成中的应用。同时,对高效固体碱催化剂设计和多过程耦合强化技术在蔗糖酯合成中的应用及其反应机制的研究进行了展望,以期为蔗糖酯的合成技术的发展提供技术指导。     

丙二醇法合成蔗糖脂肪酸酯工业性实验

进行了由蔗糖和脂肪酸乙酯在丙二醇溶剂中经酯交换合成蔗糖脂肪酸酯(Sucrose fatty acid esters)简称蔗糖酯(SE)的300 t/a工业性实验。该合成工艺用丙醇作溶剂取代国内外沿用N,N-二甲基甲酰胺有毒溶剂的SE合成方法,工艺简单,生产成本低,易于工业化生产。该工艺合成SE收率在78%以上,SE总酯质量分数在91%以上。     

无溶剂酯交换法合成蔗糖酯

本文用正交试验法确定了无溶剂酯交换法合成蔗糖酯的优化条件，并建立了产品及中间体的分析方法。     

蔗糖羧酸多酯的合成与开发进展

论述了蔗糖酯的特性,工业合成方法,蔗糖羧酸多酯的合成精制,我国蔗糖多醌的研制开发概况以及今后的展望。     

蔗糖酯的HPLC-ELSD法分离与测定

用HPLC-ELSD法分离与测定蔗糖酯,考察了蔗糖酯的HPLC-ELSD分析条件。用Hypersil C8色谱柱(250 mm,4.6 mm,5μm),以〔V(甲醇)∶V(四氢呋喃)=90∶10〕-水二元溶剂系统为流动相,梯度洗脱,流动相流速1.0 mL/m in,柱温40℃,对商品蔗糖酯和合成蔗糖酯进行了定性和定量分析。研究结果表明,在该条件下,HPLC-ELSD有效地分离了蔗糖酯产品中的蔗糖、蔗糖单酯、蔗糖二酯、脂肪酸、硬脂酸甲酯和蔗糖多酯,不但可用于蔗糖酯合成中的终点控制,而且可以对精制后的产品进行分析,从而监控产品的质量,也可用于蔗糖酯的结构鉴定,是一种连续、快速、方便、高效的蔗糖酯的定性和定量分析方法。     

蔗糖酯合成工艺改进的研究

蔗糖酯是一种有效的食品添加剂,它可由蔗糖与脂肪酸或甘油酯在碱性催化剂条件下由有机溶剂法或无溶剂法合成得到。本文叙述了蔗糖酯在无溶剂法合成中使用新型催化剂的工艺改进研究。     

蔗糖酯研制技术进展及其需求动向

本文综述了国内外合成蔗糖酯(SE)的各种方法,并对每种方法的特点、产品分布进行分析。同时概述了蔗糖酯的研制历史,产销现状及需求动向。文献收到89年9月止。     

无溶剂法合成蔗糖硬脂酸酯的工艺研究

以乙醇代替有毒的甲醇与硬脂酸在酸催化下进行反应制出了硬脂酸乙酯。以硬脂酸乙酯与蔗糖为原料在催化剂和乳化剂的作用下，进行酯交换反应合成出蔗糖硬脂酸酯。详细考察了该合成反应过程中乳化剂、催化剂用量，反应温度，原料配比，反应时间等因素对蔗糖硬脂酸酯产率的影响，得出了较佳合成工艺条件，即硬脂酸乙酯：蔗糖摩尔比为2．15：1，乳化剂与蔗糖质量比为0．1：1，催化剂与反应物料质量比为0．14：1，反应温度－120℃，压力－4．35kPa,反应时间－3.5h。以蔗糖计，蔗糖酯产率约75．2％。此外，还把蔗糖硬脂酸酯制成易挥发衍生物，建立了分析其组成的气相色谱方法。     

蔗糖脂肪酸酯的合成

以蔗糖和硬脂酸乙酯为原料合成蔗糖酯.讨论了原料配比、时间、皂含量、催化剂用量及配比对蔗糖酯得率的影响,得到最优条件：蔗糖/硬脂酸乙酯=1/0.8,反应5 h,加入6%的脂肪酸皂和7%的催化剂,乙醇钠/碳酸钾=1/4;反应温度130～135℃.     

酶催化区域选择性合成蔗糖酯的研究进展

详细综述了非水相酶催化合成蔗糖酯的研究进展。主要介绍了酶的种类、反应介质、底物性质、外加辅助手段等因素对蔗糖酯产率以及对酶区域选择性的影响。酶催化区域选择性合成蔗糖酯的难点在于蔗糖具有多个可酰化羟基及其与酰基供体的不相溶性,提出通过介质工程、底物修饰改性、外加物理场如微波和超声波辅助等改善底物相溶性,通过筛选酶、蔗糖修饰等可以得到高区域选择性的蔗糖酯。最后指出酶催化合成蔗糖酯存在的问题、发展前景等。     

High performance liquid chromatographic separation of sucrose fatty acid esters

The synthesis of sucrose fatty acid esters always results in complex mixtures. Two procedures for quantitative analysis of sucrose monoesters, respectively sucrose diesters, by means of high performance liquid chromatography on reversed-phase columns, are described. A mixture of methanol and water (85:15, v/v) was used for the separation of the monoesters, while methanol, ethyl acetate and water (65:25:10, v/v/v) was used for the separation of diesters. These methods gave information about the amount of monoesters and diesters in the product; the ratio between sucrose monopalmitate and sucrose monostearate, and the number of the most important structure isomers. A complete separation of all the possible diester products seemed to be impossible, due to the presence of more complex structure isomers. The described procedures can give important support during preparative work on sucrose fatty acid esters and also in the evaluation of these products for application purposes.     

A solvent-free synthesis of sucrose polyesters

A solvent-free reaction system is described for making sucrose polyesters (SPE) by interesterification of sucrose and long chain fatty acid methyl esters. The process avoids the usual toxic solvents by using a novel two-stage reaction sequence. In the first stage a 3:1 mole ratio of methyl esters to sucrose is reacted in the presence of potassium soaps to form a one phase melt containing mainly lower esters of sucrose. In the second stage more methyl esters are added and reacted to produce SPE in yields up to 90% based on sucrose. Sucrate ion generated in situ with alkali metal hydrides or Na-K alloy proved to be a superior catalyst for formation of sucrose esters during both stages.     

蔗糖脂肪酸酯合成新技术

蔗糖脂肪酸酯是一种国际上公认的食品添加剂,具有广泛的应用范围。蔗糖脂肪酸酯的合成路线及工艺随着人们对产品要求的提高不断改进。中科院上海有机化学所采用了生物表面活性剂作为均相催化剂,并用无溶剂法合成了蔗糖酯,使蔗糖酯的合成达到了国际先进水平。     

Enzyme‐catalyzed regioselective synthesis of sucrose‐based esters

Sucrose‐based esters are nonionic biosurfactants, which can be synthesized from the enzyme‐catalyzed esterification/transesterification of sucrose. The multi‐hydroxyl groups of sucrose and the immiscibility of sucrose with the acyl donors are the main bottlenecks in obtaining highly regioselective sucrose‐based esters. In this mini‐review, the effects of reaction conditions such as biocatalysts, design of solvent systems used as reaction media, modification and denaturation of substrates, and coupling with external auxiliary physical fields such as microwave irradiation and ultrasonic waves on the yield of sucrose esters and regioselectivity of products are highlighted. The existing problems in the field of enzymatic synthesis of sucrose esters as well as its future perspectives were pointed out. Copyright © 2011 Society of Chemical Industry     

高效液相色谱-蒸发光检测器耦合电喷雾质谱系统分析长碳链蔗糖酯

The analysis of sucrose esters with long acyl chain by improved high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD) and electrospray ionization mass spectrum (ESI-MS) is investigated. The improved HPLC-ELSD method for the separation and quantitation of commercial and synthesized sucrose esters is described. Samples are analyzed by means of a reversed-phase (RP) HPLC using a Hypersil C8 column (250 mm×4.6 mm, 5 µm particle size) with methanol-tetrahydrofuran (volume ratio of 90︰10) and water under gradient condition as the mobile phase, in which the flow rate is 1.0 ml•min－1 and the column temperature is set at 40C. This procedure provides a complete separation and determination of monoester, diester, triester and higher esters with different acyl chain lengths in each fraction by a single run, in combination with the ESI-MS technology. With this method, it is possible to determine the approximate compositions of mono- to polyesters in one analy-sis and quantitate pure positional isomers precisely using an external standard method. It is found that the method of ESI-MS cou-pling with HPLC system for the analysis of sucrose esters is straight forward, rapid and inexpensive, and can be readily applied in synthesis, purification and structure studies.     

活性炭负载固体碱催化剂催化制备蔗糖酯

采用等体积浸浈法制备活性炭负载固体碱催化剂,利用正交试验法优化催化剂制备条件,并考察了反应条件对蔗糖和亚油酸甲酯合成蔗糖酯产率的影响.结果表明,催化剂制备的优化条件为碳酸钾与活性炭质量比0.5,活生炭粒径350μm,浸渍时间3 h,煅烧温度500℃,煅烧时间3 h.以该条件下制备的活性炭负载固体碱为催化剂,在亚油酸甲酯...