Gas chromatographic analysis of ester-type surfactants by using mixed anhydride reagent

Polyoxyethylene alkyl ether sulfates, polyoxyethylene alkyl ether phosphates, and polyoxyethylene fatty acid ester-type surfactants have been analyzed by gas chromatography after chemical decomposition by using the mixed anhydride of acetic and p-toluene-sulfonic acids. In this way, the hydrophobic groups of the polyoxyethylene alkyl ether sulfates and polyoxyethylene alkyl ether phosphates can be identified in the form of alkyl acetates, and the alkyl compositions can be determined easily. On the other hand, the hydrophobic groups of the polyoxyethylene fatty acid ester-type surfactants, such as polyoxyethylene fatty acid ester, polyoxyethylene glycerol fatty acid ester, and polyoxyethylene sorbitan fatty acid ester, have been identified after conversion into their corresponding fatty acids. At the same time, the base compounds of the hydrophilic groups have been converted into ethylene glycol diacetate, glycerol triacetate, and isosorbide diacetate, respectively, so these surfactants may be distinguished easily.     

醇醚型表面活性剂疏水基和分子量的测定

用＾１３Ｃ－ＮＭＲ技术测定了醇醚型表面活性剂基Ｒ的平均碳数、环氧乙烷平均合数和平均分子量,并用实例说明了测量方法与步骤。最后列出了不同试样的分析结果,并与以谱联合 Ｈ－ＮＭ法测得的结果进行了比较,得到了满意的结果。     

新型非离子型自乳化水性环氧树脂固化剂的合成与表征

采用十八胺与乙二醇二缩水甘油醚反应,制得一种两端为环氧基,中间氮原子上接有长疏水烷基链的功能性双环氧基化合物,再用脂三乙烯四胺对该化合物进行封端,制得一种非离子型水性环氧固化剂.研究表明:由于该固化剂具有疏水效果的长烷基链和亲水效果的羟基、胺基、醚键,从而使得该固化剂具有表面活性剂的结构.因此相对其他水性固化剂来讲,该固化剂不仅仅不需要采用中和剂就具有亲水性,且其对环氧树脂有良好的乳化效果.该固化剂与液体环氧树脂所制备的双组分室温固化涂膜性能优良,具有优异的铅笔硬度、耐冲击性和耐化学性.同时该固化剂含有较长的柔性烷基链,所以固化后的环氧树脂将有较好的柔韧性.     

烷基酚聚氧乙烯醚的定性分析

利用氢碘酸作裂解剂处理烷基酚聚氧乙烯醚试样 ,采用气相色谱 质谱联用技术对其进行定性分析。根据气相色谱图及质谱检测得到的特征峰分析其组成 ,可得知油剂中的未知组分     

液晶显示器清洗剂配方开发

在以脂肪醇聚氧乙烯甲基醚、脂肪醇聚氧乙烯聚丙烯醚、脂肪醇聚氧乙烯醚、乙醇胺、乙二醇丁醚、乙二胺四乙酸为主要原料制备的清洗剂配方中,研究了脂肪醇聚氧乙烯醚、乙醇胺、乙二醇丁醚的用量对清洗剂清洗效果的影响。通过正交试验优化了实验参数,得到了所选水平下的最佳配方:脂肪醇聚氧乙烯醚用量为5%,乙醇胺用量为5%,乙二醇丁醚用量为15%。该配方下清洗剂的泡沫较少,碱性较强,清洗效果最佳。     

Preparation and surface activity of gelatin‐derived surfactants modified with polyoxyethylene stearyl ether units

We have prepared a series of novel gelatin derivatives through reactions of gelatin with alkyl succinic anhydride and polyoxyethylene stearyl ether. These derivatives contain gelatin units and polyoxyethylene chains as their hydrophilic moieties and alkyl succinic anhydrides and 18‐carbon‐atom alkyl chains as their hydrophobic moieties. Surface activities were evaluated in terms of the materials' surface tensions, wetting abilities, emulsifying powers, and foaming properties. The surface tensions were characterized with respect to the critical micelle concentration (cmc), the surface tension at the cmc, the maximum surface excess concentration, the standard free energy, and the surface area per molecule at the air‐water interface. The modified gelatins were more surface‐active relative to gelatin itself. Increasing the polyoxyethylene chain length led to a decrease in surface activity. The excellent foaming, wetting, and emulsifying behavior of the gelatin derivatives was a direct result of the presence of their multiple hydrophilic and hydrophobic units. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

窄分布醇醚下游衍生产品的差异化

论述了窄分布脂肪醇(聚氧乙烯)醚的研究进展,从物化性能、合成及应用、国内外发展概况等方面重点介绍了脂肪醇醚羧酸盐(AEC)、脂肪醇醚磺基琥珀酸酯二钠盐(AESS)和脂肪醇醚磷酸酯(MAEP),展望了窄分布醇醚下游衍生产品的发展前景。     

Influence of dialkyl ethers on the surface properties of homogeneous nonionic surfactants

Influence of the trace amounts of the corresponding dialkylethers on the surface and colloidal properties of the pure polyoxyethylene alkyl ethers were studied. The dialkyl ether, undetected by gas liquid chromatography (GLC) was found by gel permeation chromatogram (GPC) as the corresponding impurity in homogeneous pure polyoxyethylene alkyl ether and confirmed using infrared (IR), nuclear magnetic resonance (NMR) and mass spectroscopy (MS). After removing the corresponding impurity in each surfactant with a GPC separation column, the minima in the surface tension curves disappeared completely. Adding the corresponding dialkyl ether to the pure surfactant produced the minima in the surface tension curves and large values for surface aging, cloud points were lowered more than for the pure surfactants and foam height and foam stability for the aqueous solutions decreased gradually.     

潜伏型非离子自乳化环氧固化剂的合成与性能

采用十八胺与乙二醇缩水甘油醚为原料,制得了一种两端为环氧基、中间氮原子上接有长疏水烷基侧链的双环氧基化合物,再用酮亚胺上剩余的仲胺对该化合物进行封端,制备了潜伏型的非离子自乳化环氧固化剂;并用红外光谱验证了每一步的产物。该固化剂在水环境下,释放出具有亲水功能的氨基,再加上分子本身具有亲水功能的羟基、醚键和疏水功能的长烷基侧链,该固化剂兼具固化功能和乳化功能。所制备的水性环氧树脂涂料具有良好的柔韧性能、铅笔硬度、附着力、透明性和耐水性。     

低加成数脂肪醇聚氧乙烯醚的气相色谱分析

采用HP4890毛细管色谱柱、程序升温、FID检测，较好的分离了各种低加成数脂肪醇聚氧乙烯醚（AEO）样品中的各组分；使用GC－MS进行了样品中组分的定性，并经实验研究彩和峰面积归一化法进行了组分的定量，较准确地计算出了各种样品AEO游离脂肪醇质量分数及聚氧乙烯醚的环氧乙烷（EO）加成数分布。方法简便、快速，有较好的准确度和精确度。     

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。     

二脱水山梨醇聚氧乙烯醚油酸酯纯品的合成

山梨醇经催化脱水,高真空减压蒸馏得到二脱水山梨醇,与环氧乙烷反应得到二脱水山梨醇聚氧乙烯醚,最后与高纯度油酸缩合得到高纯度组分二脱水山梨醇聚氧乙烯醚油酸酯,是聚山梨酯80的重要组成成分。     

Preparation and Surface Activities of Modified Double-Tailed Anionic Surfactants

We prepared a series of modified double-tailed surfactants containing two identical nonionic moieties and an anionic spacer group. Each surfactant was prepared through the reaction of two moles of polyoxyethylene alkyl ether with one mole of maleic anhydride to form a diester having a gemini structure; an anionic sulfonate group was then introduced through reaction of the olefinic bond with sodium hydrogen sulfite. The structures of these compounds were confirmed through infrared spectroscopy, nuclear magnetic resonance spectroscopy, and elemental analysis. These modified double-tailed surfactants exhibit good surface properties, including low-foaming, wetting and lime-soap dispersing power. Their excellent dispersing abilities toward disperse dyes were due to the double-tailed structures of the surfactants, with the hydrophobic moieties increasing the binding ability to the dyes and its anionic units providing dispersing power.     

Well-defined multi-stimuli responsive fluorinated graft poly(ether amine)s (fgPEAs)

Well-defined multi-stimuli responsive fluorinated graft poly(ether amine)s (fgPEAs) were synthesized through nucleophilic substitution/ring-opening reaction of commercial poly(propylene glycol) diglycidyl ether and Jeffamine L100, followed by functionalization of hydroxyl groups in backbone by fluorinated alkyl carboxylic acid. fgPEAs are comprised of hydrophilic short poly(ethylene oxide) (PEO) and hydrophobic fluorinated alkyl chains, which are grafted on poly(propylene oxide) (PPO) backbone alternately to form well-defined structure. In aqueous solution, fgPEA11 and fgPEA12 self-assembled into multi-dispersed micelles, while fgPEA13 formed the uniform-sized micro-micelles with diameter of about 200 nm. These obtained micelles from fgPEAs were multi-responsive to temperature, pH and ionic strength with tunable cloud point (CP). It’s notable that CP of fgPEAs aqueous solution increased with the increasing amount of graft fluorinated alkyl chains.     

Microemulsion polymerization of siloxane with nonionic surfactants as emulsifiers

Polysiloxane nanolatices were prepared by the microemulsion polymerization of octamethylcyclotetrasiloxane (D₄) with nonionic polyoxyethylene alkyl ether and polyoxyethylene aryl ether as surfactants, ethylene glycol or aminoethanol as a cosurfactant, and potassium hydroxide or dipotassium dimethylsilanolate (I) as an initiator. The effect of the different initiators and the amount of cosurfactant on the microemulsion polymerization rate of D₄ was investigated. The initiator, potassium hydroxide, had a similar catalytic activity to I, and adding the cosurfactant changed a common siloxane emulsion to a microemulsion. At a same reaction conditions, the polymerization rate of D₄ with aminoethanol as a cosurfactant was much faster than that of ethylene glycol. The kinetics of this siloxane microemulsion polymerization was consistent with Morgen‐Kaler theory. The transparency value of the resultant polysiloxane nanolatex was more than 95% when the amount of ethylene glycol was more than 25% and the siloxane amount was about 30 wt % of the reaction mixture. A nanolatex of polydimethylsiloxane‐co‐polyvinylmethylsiloxane, which was crosslinked with potassium persulfate, revealed that the mean diameter of the droplets was 32 nm with a narrow distribution. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 3587–3593, 2003     

一种环保型乳化剂复配体系的研究

研究了淀粉糖苷非离子表面活性剂与脂肪醇聚氧乙烯醚硫酸酯钠盐阴离子型表面活性剂、脂肪醇聚氧乙烯醚非离子表面活性剂的混合体系的乳化力的变化规律,找出复配体系的最佳配方,将其乳化性与常用的烷基酚聚氧乙烯(10)醚进行比较。结果表明,复配后的体系有较低的表面张力,对菜油的乳化性与烷基酚聚氧乙烯(10)醚相当,对变压器油的乳化性优于烷基酚聚氧乙烯(10)醚。且该体系浊点高,泡沫稳定,乳化性能好。     

双功能改性丙烯酸树脂皮革涂饰剂的研制

在丙烯酸丁酯—丙烯腈—丙烯酸甲酯体系中，引入１％～２％的丙烯酸，２％～３％的Ｎ－羟甲基丙烯酰胺，５％的烷基酚聚氧乙烯醚硫酸铵与十二烷基硫酸钠复配乳化剂，采取自生种子聚合技术可制得双功能团改性的丙烯酸树脂皮革涂饰剂。     

脂肪醇聚氧乙烯醚系列磺酸盐的泡沫性能研究

磺酸盐类阴离子表面活性剂在采油工业中应用广泛,其泡沫性能(起泡性和泡沫稳定性)对采收率影响很大。采用改进的Ross-Miles法对烷基碳数为14、16、18的脂肪醇聚氧乙烯(3)醚磺酸钠(CnH2n 1O(EO)2CH2CH2SO3Na,n=14、16、18)在不同条件下的泡沫性能进行了研究。结果表明,随着疏水基长度增加,表面活性剂起泡性降低,稳泡性增强;十四醇聚氧乙烯(3)醚磺酸钠起泡性最好,十八醇聚氧乙烯(3)醚磺酸钠稳泡性最优;随着温度的上升,3种表面活性剂起泡性增强,稳泡性降低。     

涤纶POY油剂单体的合成及性能研究

以碳酸二乙酯为原料,与丙二醇聚醚反应,合成了低级聚碳酸酯,再用自制的不同脂肪醇聚氧乙烯醚封端,合成了改性聚碳酸酯;将改性聚碳酸酯与其他单体复配,配制成涤纶POY油剂,考察脂肪醇聚氧乙烯醚的起始剂、环氧乙烷(EO)与环氧丙烷(PO)加成数,碳酸二乙酯与丙二醇聚醚的摩尔比对POY油剂性能的影响。结果表明:使用辛醇为起始剂,与EO按摩尔比1:8缩合合成脂肪醇聚氧乙烯醚,1,2-丙二醇与PO按摩尔比1:8缩合合成丙二醇聚醚,碳酸二乙酯与丙二醇聚醚按摩尔比4:3缩合成低级聚碳酸酯,低级聚碳酸酯与脂肪醇聚氧乙烯醚按摩尔比1:1合成的改性聚碳酸酯作为单体复配的涤纶POY油剂,其润湿性能、热性能较好,表面张力较高。     

非离子型腈纶油剂的研制

以4-仲丁基-2,6-二叔丁基苯酚、环氧乙烷为原料,KOH为催化剂,合成4-仲丁基-2,6-二叔丁基苯酚聚氧乙烯醚抗静电剂,与山梨醇单硬脂肪酸酯、蓖麻油聚氧乙烯醚、十二胺醚等表面活性剂复配成非离子型腈纶油剂。结果表明:上油后的腈纶短纤维的质量比电阻为2.1×10~8Ω·g/cm~2,摩擦系数适中,能满足腈纶生产和加工要求。