脂肪酸烷醇酰胺酯类表面活性剂的研究进展与发展趋势

详细介绍了脂肪酸烷醇酰胺硫酸酯、脂肪酸烷醇酰胺磷酸酯、脂肪酸烷醇酰胺硼酸酯三大类脂肪酸烷醇酰胺酯类表面活性剂的合成方法、表面性能及应用领域的研究现状,并展望了其研究开发方向及应用发展趋势。     

烷醇酰胺衍生物类表面活性剂的研究进展

本文综述了近年来脂肪酸烷醇酰胺衍生物类表面活性剂的研究现状,详细介绍了烷醇酰胺磷酸酯、烷醇酰胺醚羧酸盐、烷醇酰胺硫酸酯、烷醇酰胺硼酸酯等几类表面活性剂的合成方法、表面性能及应用领域,并指出该类表面活性剂因其优良的表面活性和良好的生物降解性具有广阔的发展前景。     

脂肪酸烷醇酰胺磷酸酯表面活性剂的合成及性能研究

以C14~18的脂肪酸与二乙醇胺反应合成了系列脂肪酸烷醇酰胺,再经磷酸化反应及中和反应制备了6种脂肪酸烷醇酰胺磷酸酯盐表面活性剂。分别测定了各产物的组成及表面活性,考察了无机盐对表面张力(γ)及临界胶束浓度(cmc)的影响,测试了不同碱中和产物水溶液与系列烷烃间的界面张力。结果表明,脂肪酸碳数为14,16和18的烷醇酰胺磷酸酯盐表面活性剂的cmc分别为50,50和30 mg/L,γcmc为26~31 mN.m-1;无机盐对产物的cmc影响不大;在质量分数为0.3%时,6种表面活性剂水溶液与正构烷烃形成最低界面张力的最小烷烃碳数为10~16,其中用NaOH中和得到的C14N与十二烷、十四烷以及C16N与十六烷均可达到超低界面张力,分别为0.007 8,0.008 3和0.001 6 mN.m-1,用二乙醇胺中和得到的C14D也可与癸烷达到超低界面张力。     

米糠油与二乙醇胺制备烷醇酰胺

采用资源丰富的米糠油与二乙醇胺反应制备了米糠油烷醇酰胺。其主要工艺参数：原料配比为米糠油脂肪酸：二乙醇胺=1：2，氮气1～1.2kg/cm~2；反应时间3～10h；催化剂氢氧化钾为总量的0.5％。产品得率为95～97％。测定了产物的表面性能和与某些阴离子表面活性剂的配伍性能。表明制得的米糠油烷醇酰胺与椰子油烷醇酰胺的性能基本相同。     

天然油脂脂肪酸甲酯及其酰胺衍生物的合成

本文以天然油脂为原料,采用正交试验的方法,合成制得脂肪酸甲酯,并和二乙醇胺进行酰胺化反应得到脂肪酸烷醇酰胺型非离子表面活性剂,为其进一步的研究奠定了基础。     

以地沟油制备烷醇酰胺的研究

以地沟油为原料,采用甲酯法生产烷醇酰胺表面活性剂。利用两步酸碱酯交换法使地沟油转化为生物柴油,生物柴油在氢氧化钠催化作用下与二乙醇胺反应生成烷醇酰胺。探讨了生物柴油合成烷醇酰胺的最佳合成条件。结果表明,在生物柴油与二乙醇胺的摩尔比为1∶1.6,催化剂氢氧化钠用量为生物柴油质量的0.8%,反应温度110℃,反应时间2 h,真空度0.09 MPa条件下合成烷醇酰胺,产率可达95.64%,产品具有优良的表面活性。     

菜籽油烷醇酰胺的合成及性能测定

以菜籽油脂肪酸甲脂为原料,分别与乙醇胺和二乙醇胺在碱性条件下反应,合成脂肪酸单乙醇酰胺、1∶1型脂肪酸二乙醇酰胺和1∶2型脂肪酸二乙醇酰胺,并对这三种烷醇酰胺进行系统的性能测试。结果表明由菜籽油脂肪酸甲脂合成的脂肪酸单乙醇酰胺的胺值低、乳化性好和cmc低,但起泡性、润湿性和钙皂分散力较差;1∶1型脂肪酸二乙醇酰胺乳化性和钙皂分散力较好,但水溶性和起泡性较差;1∶2型脂肪酸二乙醇酰胺乳化效果差,胺值高,但起泡性和润湿性较好。三种烷醇酰胺性能不尽相同,为表面活性剂开发和生物柴油的综合利用探索了一条新的途经。     

以地沟油制备烷醇酰胺的研究

以地沟油为原料,采用甲酯法生产烷醇酰胺表面活性剂。利用两步酸碱酯交换法使地沟油转化为生物柴油,生物柴油在氢氧化钠催化作用下与二乙醇胺反应生成烷醇酰胺。探讨了生物柴油合成烷醇酰胺的最佳合成条件。结果表明,在生物柴油与二乙醇胺的摩尔比为1∶1.6,催化剂氢氧化钠用量为生物柴油质量的0.8%,反应温度110℃,反应时间2 h,真空度0.09 MPa条件下合成烷醇酰胺,产率可达95.64%,产品具有优良的表面活性。     

从米糠油合成洗涤用品

利用资源丰富的米糠油(RBO)作为制备新型阴离子表面活性剂的原料,原料油脂经水解成游离脂肪酸,再磺化至α—磺基脂肪酸及其相应的盐作为洗涤剂的组份。将米糠油进行工业条件氢化代替牛油,作为肥皂工业硬脂原料,也可将米糠油脂肪酸与二乙醇胺反应,制备与椰子油烷醇酰胺性质相同的非离子表面活性剂。     

N-十六烷基硼酸二乙醇胺酯的合成及其表面活性研究

以二乙醇胺与硼酸酯化合成二乙醇胺硼酸酯(Ⅰ),Ⅰ再与1-溴代十六烷烷基化合成一类新型的含硼两性表面活性剂N-十六烷基硼酸二乙醇胺酯(Ⅱ).反应条件为以无水乙醇为溶剂n(Ⅰ)∶n(1-溴代十六烷)∶n(Na2CO3)＝1∶1∶1,80 ℃反应8 h,收率达88.0%.两步总收率达80.1%.产物通过红外和核磁确定.考察了pH值和盐度对表面张力的影响.     

一种新型气相色谱固定液的制备及应用

以柠檬酸、OP-10和二乙醇胺为原料合成了柠檬酸壬基酚聚氧乙烯醚单酯二乙醇酰胺。用红外光谱法表征了结构,热分析技术考察了热稳定性。以此产物作为气相色谱固定液,对一些混和组分进行分离,效果良好。     

聚乙二醇600油酸酯作为气相色谱固定液的研究与应用

本文用聚乙二醇600和油酸合成了聚乙二醇600油酸酯非离子型表面活性剂，精制后作为气相色谱固定液，制备成色谱柱。测定此固定液的最高使用温度、相对极性。对一些混合物组分的分离效果表明了此固定液具有良好的应用性能，是一种新型的气相色谱固定液。     

Synthesis and purification of trisulphoindigo and reversed-phase high performance liquid chromatographic determination of trisulphoindigo in FD & C Blue No.2

The effect of temperature on product formation during the sulphonation of indigo with concentrated sulphuric acid and 30 % fuming sulphuric acid was studied with the aid of high performance liquid chromatographic (HPLC) analysis. Trisulphoindigo was prepared by the sulphonation of indigo with concentrated sulphuric acid at 160°C. The di- and tetra-sulphoindigo side products formed during the reaction were removed by preparative HPLC to yield a product of high chromatographic purity. The trisulphoindigo content of the food dye FD & C Blue No. 2 and the purity of commercially available trisulphoindigo were determined by HPLC analysis.     

Chiral separation by combining pertraction and preferential crystallization

This work describes the application of a hybrid two-step enantioselective separation process. As a first step, pertraction using supported liquid membranes provides an initial enrichment, while the following preferential crystallization delivers the enantiopure crystals as final product. Mandelic acid in water was studied as a model system. Using a suitable chiral selector, pertraction provides enrichments exceeding 10% and reaching up to 20% in the permeate phase, which was sufficient to allow for subsequent selective preferential crystallization. Based on the individual performances of pertraction and crystallization, overall yields and productivities are estimated. The calculated productivities are compared with values achievable in alternatively applicable chromatographic separation processes using chiral stationary phases. The realized hybrid pertraction-crystallization process is in its present state for the example considered still inferior to preparative chromatography. Strategies for further improvement are suggested.     

草酸二甲酯和草酸的反相高效液相色谱分析

建立了反相高效液相色谱定量分析草酸二甲酯生产过程中的草酸二甲酯及草酸含量的方法。采用带有紫外检测器的Shimadzu LC-20A型高效液相色谱仪,C18色谱柱(4.6 mm×150 mm,5 μm),流动相是体积比为60:40的乙腈-磷酸水溶液(pH=2.7),流速为0.7 mL/min,柱温25 ℃,254 nm波长下紫外检测。探讨了pH值及其它条件对色谱分离的影响。该方法测得的草酸及草酸二甲酯线性回归曲线的相关系数分别为0.9996和0.9998,相对标准偏差为0.8%~1.0%,满足定量分析要求。     

A Comparison of Dicoronylene and Octadecylsilica Stationary Phases for Separation of Polycyclic Aromatic Hydrocarbons by Microcolumn Liquid Chromatography

The chromatographic performance of dicoronylene as a stationary phase in microcolumn liquid chromatography has been investigated. The performance has been compared to commercially available polymeric and monomeric octadecylsilica stationary phases. Similarities between polymeric octadecylsilica phases and dicoronylene are found in their planarity recognition capability for polycyclic aromatic hydrocarbons. This is explained by the planar structure of dicoronylene being able to recognize planar solutes in the liquid chromatographic environment, as explained by the “slot model” as proposed by Wise et al.     

氟喹诺酮类药物沙拉沙星分子印迹聚合物的制备

本文采用本体聚合法,以沙拉沙星为模板分子合成了沙拉沙星分子印迹聚合物,并用高效液相色谱法研究了印迹聚合物的识别性能及作为色谱固定相的分离及影响因素,该固定相对模板分子有较好的的特异性识别能力。     

单分散高分子微球的制备及色谱性能考察

以二乙烯基苯(DVB-55)和二乙二醇二甲基丙烯酸酯(DGD)为共聚单体,采用沉淀聚合法在乙腈溶剂中一步制得了聚(二乙烯基苯-co-二乙二醇二甲基丙烯酸酯)微球[P(DVB-DGD)]。用FTIR、SEM和BET等方法对P(DVB-DGD)进行表征,结果表明,两种单体在聚合过程中实现了共聚,数均粒径为3.6μm的单分散微球表面未见大孔结构,微球比表面积为2.9 m2/g,平均孔径为9.1 nm。以两组试样为探针分子,采用反相液相色谱模式考察了P(DVB-DGD)填充的新型固定相的色谱性能,结果显示,组分获得了尖锐对称的峰形。色谱柱呈现了较高柱效和良好色谱性能,表明沉淀聚合在HPLC固定相方面具有较好应用前景。     

离子液体在色谱分析中的应用

综述了近年来国内外离子液体在色谱分析中的应用情况,主要包括离子液体用作气相色谱固定相,液相色谱流动相或流动相添加剂,以及毛细管电泳电解质、添加剂或涂布于毛细管壁上分离各种物质。     

Supramolecular Chromatographic Separation of C60 and C70 Fullerenes: Flash Column Chromatography vs. High Pressure Liquid Chromatography

A silica-bound C-butylpyrogallol[4]arene chromatographic stationary phase was prepared and characterised by thermogravimetric analysis, scanning electron microscopy, NMR and mass spectrometry. The chromatographic performance was investigated by using C₆₀ and C₇₀ fullerenes in reverse phase mode via flash column and high-pressure liquid chromatography (HPLC). The resulting new stationary phase was observed to demonstrate size-selective molecular recognition as postulated from our in-silico studies. The silica-bound C-butylpyrogallol[4]arene flash and HPLC stationary phases were able to separate a C₆₀- and C₇₀-fullerene mixture more effectively than an RP-C₁₈ stationary phase. The presence of toluene in the mobile phase plays a significant role in achieving symmetrical peaks in flash column chromatography.