HPLC-MS法测定纺织染整助剂中烷基酚及烷基酚聚氧乙烯醚

本文采用高效液相色谱-质谱法检测了纺织染整助剂产品中烷基酚及烷基酚聚氧乙烯醚,包括辛基酚(OP)、壬基酚(NP)、辛基酚聚氧乙烯醚(OPEO)、壬基酚聚氧乙烯醚(NPEO)。对样品前处理方法进行了优化和选择。     

GC/MS测定水体中烷基酚及烷基酚聚氧乙烯醚的方法研究

文章采用二氯甲烷对水体样品进行液液萃取后加入BSTFA+TMCS进行衍生,结合气相色谱/质谱联用的方法测定水体中的烷基酚(壬基酚、辛基酚、对-特-辛基苯酚)、短链壬基酚聚氧乙烯醚、短链辛基酚聚氧乙烯醚。方法在0.5~50 mg/L范围内线性良好,目标化合物的检出限为1 ug/L。     

烷基酚、烷基酚聚氧乙烯醚的测定方法验证

通过对我检测实验室烷基酚、烷基酚聚氧乙烯醚检测方法的测试能力进行检测，方法验证结果表明，我实验室有检测样品中烷基酚、烷基酚聚氧乙烯醚的能力和资源。     

高效液相色谱-质谱法测定车用清洗剂中烷基酚聚氧乙烯醚

建立了一种用于检测车用清洗剂中烷基酚聚氧乙烯醚的高效液相色谱-质谱法。流动相采用5 mmol/L乙酸铵和甲醇混合溶液,采用梯度淋洗模式,色谱柱柱温为40℃,流速为0.3 mL/min,进样量为10μL,质谱检测器为电喷雾离子源(ESI),采用选择离子(SIM)正模式。该法所建立的辛基酚聚氧乙烯醚(OPEO)和壬基酚聚氧乙烯醚(NPEO)的线性范围分别为1.0~50.0和0.5~50.0 mg/L,线性系数r均大于0.999,辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的方法检出限分别为1.0和0.5 mg/kg,精密度分别为1.5%和2.8%(n=8),加标回收率分别为80.0%~98.3%和88.5%~100.2%。该方法操作简单、准确、快捷,可用于车用清洗剂中辛基酚聚氧乙烯醚及壬基酚聚氧乙烯醚的定性与定量检测。     

烷基酚的性质及应用

烷基酚是精细化工生产中的重要中间体之一,它被广泛应用于表面活性剂、橡胶和塑料用的抗氧剂、合成烷基酚树脂及烷基酚磷酸脂等生产领域。烷基酚可由烯烃、脂肪醇或氯代烃与苯酚经烷基化反应生成,但工业上重要的烷基酚是由苯酚和烯烃在催化剂作用下制得的。对-叔丁基酚、对-叔辛基酚、对-特壬基酚和十二烷基酚都是最重要的烷基酚。目     

液相色谱-串联质谱法测定洗涤用品中的烷基酚

研究并建立了洗涤用品(液类、粉类和皂类)中4种烷基酚(对叔辛基酚、邻正壬基酚、对正辛基酚、对正壬基酚)的液相色谱-串联质谱的检测分析方法。洗涤用品样品以甲醇为提取溶剂,超声提取,过膜,滤液上机测量。采用Waters XBr idge C18色谱柱,以甲醇-0.1%氨水溶液为流动相,梯度洗脱分离后,在LC/MS/MS多反应监测模式下进行定性与定量分析。对叔辛基酚、邻正壬基酚、对正辛基酚和对正壬基酚定量限分别为1、1、0.5和0.5μg/kg,4种烷基酚线性范围均为0.2~100μg/kg;皂类洗涤用品中4种烷基酚在低、中、高3种加标水平的回收率为83.1%~117.4%,相对标准偏差为2.1%~10.3%;液类洗涤用品中4种烷基酚在低、中、高3种加标水平的回收率为82.2%~116.3%,相对标准偏差为1%~8.1%;粉类洗涤用品4种烷基酚中,对叔辛基酚、邻正壬基酚、对正辛基酚3种在低、中、高3种加标水平的回收率为81.8%~114.6%,而对正壬基酚添加回收率仅为44.9%~55.1%,4种烷基酚相对标准偏差为1.4%~7.1%。应用该方法对市面上销售的洗涤产品进行了检测,并对结果进行了分析。     

烷基酚聚氧乙烯醚的环境行为和环境风险评价

烷基酚聚氧乙烯醚（APEOs)的生物降解中间体短碳链的烷基酚聚氧乙烯醚（APEOn,n=1,2),烷基酚聚氧乙烯醚酸酯（n=1,2)和烷基酚（AP）更耐降解,AP和APEOn主要吸附于污泥,APEnC主要存留在水体。河水中APEOs代谢物的浓度远低于水生物急剧毒性的最低限,研究还发现一些烷基酚类化合物具雌性激素活性。     

烷基酚聚氧乙烯醚的毒性和法规现状（英）

介绍了国际上有关烷基酚聚氧乙烯醚的生物降解性，毒性，使用和限制法规情况。尽管有关烷基酚聚氧乙烯醚的生物降解性和毒性问题尚未有定论，大部分国家没有使用的法规，但发达国家已在家用洗涤剂中自发地停止使用，工业洗涤也已开始自发地停止使用，发展中国家还在继续使用。     

烷基酚聚氧乙烯醚的安全性问题

烷基酚聚氧乙烯醚（APEO）是广泛使用的表面活性剂。按照欧盟法则2003／53／EG,从2005年1月17日起欧洲对APEO的使用进行了严格的限制。介绍了烷基酚聚氧乙烯醚的生物降解性、生态毒性效应及其环境行为等,并指出必须加大替代品的研究和开发力度。     

复合多烷基酚聚氧乙烯醚开发研究

本文介绍了以辛烷基酚生产过程产生的“下脚”,多烷基酚高沸物为原料,通过与不同摩尔数的环氧乙烷缩合;不同调节剂及复合用量的选择,开发出适用作聚酯纤维高温印染工艺的匀染剂,复合多烷基酚聚氧乙烯醚。     

Sulfates of ethoxylated tridecyl alcohol in dishwashing formulations

Summary The foam stability of several light-duty liquid dishwashing formulations containing sulfated ethoxylates of tridecyl alcohol, lauryl alcohol, and nonylphenol have been compared. The effects of water hardness, sulfating agent, and ethylene oxide/hydrophobe mole ratio have been examined. In very soft water formulations containing alkanolamide and tridecyl alcohol derivatives were shown to be especially effective. At higher water-hardnesses, combinations containing sulfated ethoxylates of tridecyl alcohol and nonylphenol performed best. Optimum ethylene oxide content for the sulfated tridecyl alcohol ethoxylates has been shown to be 4 to 5 moles/mole of alcohol regardless of water hardness or detergent concentration. The alcohol ethoxylates were shown to be more tolerant of stronger sulfating agents with respect to product quality than the alkylphenol ethoxylates. Presented at the fall meeting, American Oil Chemists’ Society, Los Angeles. Calif., Sept. 28–30, 1959.     

光催化降解壬基酚聚氧乙烯醚的研究

研究了以悬浮态TiO2为催化剂,在H2O2存在的条件下,对壬基酚聚氧乙烯醚的光催化降解反应。分别考察了pH值、TiO2和H2O2的加入量、壬基酚聚氧乙烯醚的初始浓度以及光照时间对降解反应的影响。结果表明:在pH值为5,H2O2质量浓度为30mg/L的条件下,对初始质量浓度为50mg/L的壬基酚聚氧乙烯醚溶液光照4h后降解率达46.32%。     

Analysis of nonionic surfactants in bench-scale biotreater samples

The effluents and activated sludges used in benchscale biotreater units have been analyzed for nonionic alcohol ethoxylates and their residues. Separate bench-scale units were fed linear alcohol ethoxylates (AE), highly branched and branched nonylphenol ethoxylates. Effluents and sludges were first pretreated by a foam sublation technique to provide a gross separation of surfactants from the environmental matrix. This step was followed by normal-phase high-performance liquid chromatography (HPLC) with either fluorescence detection (FD) or evaporative light-scattering detection (ESLD). The AEs were derivatized with phenylisocyanate and analyzed by normal-phase HPLC coupled with FD. At extremely low surfactant levels, pretreatment of large sample volumes resulted in interferences on derivatization. Hence, a normal-phase HPLC method with ELSD was developed. Although some interferences do appear using ELSD, this method appears to be a more viable alternative to derivatization/FD for very low levels of AE. HPLC with FD and ELSD detection methods are more quantitative and provide information on the polyoxyethylene chain than is possible with traditional methods like cobalt-thiocyanate active substance. Presented at the 82nd AOCS Annual Meeting & Expo, May 1991, Chicago, Illinois.     

壬基环己醇聚氧乙烯醚硫酸盐的合成及性能

壬基酚聚氧乙烯醚硫酸钠因具有水生毒性而亟需开发其替代物。壬基环己醇聚氧乙烯醚由于其安全性较高,且理化性能与壬基酚聚氧乙烯醚的接近,是壬基酚聚氧乙烯醚潜在的替代物。本文以壬基环己醇聚氧乙烯醚为原料,氯磺酸为硫酸酯化试剂,合成了壬基环己醇聚氧乙烯醚硫酸钠,其中壬基环己醇聚氧乙烯醚（5）硫酸钠和壬基环己醇聚氧乙烯醚（9）硫酸钠（5, 9分别为其环氧乙烷加成数）的酯化率分别可达90.91% 和91.06%。壬基环己醇聚氧乙烯醚（5）硫酸钠水溶液与脂肪醇聚氧乙烯醚（3）硫酸钠（AES）具有相近的表界面活性。合成产物壬基环己醇聚氧乙烯醚硫酸钠具有和壬基环己醇聚氧乙烯醚相当的润湿及泡沫性能,比AES更好的润湿、泡沫及乳化性能。     

利用伪三元相图法制备1O0％咪鲜胺微乳剂

在配方初步筛选表面活性剂的基础上,非离子表面活性剂-壬基酚聚氧乙烯醚和阴离子表面活性剂-的十二烷基苯磺酸钙。通过两者不同的配比,绘制出10％咪鲜胺微乳体系的伪三元相图,利用相图确定乳化剂最佳配比的合适配方,并检测了微乳剂样品的物理稳定性。最终配方为：咪鲜胺10％,壬基酚聚氧乙烯醚18％,十二烷基苯磺酸钙2％,异丙醇10％,水余量。     

新型表面活性剂在洗衣液中的应用

洗衣液市场的快速增长促进了其技术的不断进步与产品创新。从洗衣液技术发展趋势的角度讨论了脂肪酸甲酯磺酸盐(MES)、仲烷基磺酸盐(SAS)、异构醇聚氧乙烯醚、脂肪醇聚氧乙烯-聚氧丙烯醚以及脂肪酸甲酯乙氧基化物等新型表面活性剂在洗衣液中的应用和发展前景。     

Application of Green Commercial Surfactant in Preparing Purely Acrylic Latex via Semi-continuous Seeded Emulsion Polymerization

Nonylphenol ethoxylates (NPEOs) are widely used as surfactants for emulsion polymerization and for post adding stabilization for latex applications in formulations with high filler content. However, NPEOs are bioaccumulative and persistent in the environment while nonylphenol, the breakdown product of NPEs, is an endrocrine disruptor. Therefore, it has been recommended to ban technical processes using NPEOs as surfactants. The acrylic polymer latex was prepared via semi-continuous seeded emulsion polymerization of butyl acrylate and methyl methacrylate in water phase initiated with potassium persulfate when nonylphenol ethoxylates are replaced with alkyl polyglycoside (APG) surfactants. The structure of the resultant acrylic polymer latex is confirmed with Fourier transform infrared spectroscopy spectrum. Differential scanning calorimetry confirms that the resultant latex is a kind of random copolymer and the consistency among the chain segment is fairly good. Influences of amount of APG on the properties of the resultant latex and its film were investigated. Results show that the particle size of the latex is decreased with the increase of the amount of APG. And the ionic stability of latex is also improved with the increase of the amount of APG. However, the water-resistance of the film of the latex is decreased with the increase of the amount of APG.     

可聚合乳化剂合成含氟丙烯酸酯无皂乳液及其性能

以甲基丙烯酸甲酯（MMA）、丙烯酸丁酯（BA）、甲基丙烯酸六氟丁酯（HFMA）等为主要原料,采用预乳化种子乳液聚合法合成了含氟丙烯酸酯无皂乳液,考察了可聚合乳化剂烯丙氧基壬基酚聚氧乙烯（10）醚硫酸铵（DNS-86）和HFMA的用量对无皂乳液的电解质稳定性和涂膜耐水性的影响。利用傅里叶红外光谱、差示量热扫描仪及热重分析对氟丙乳液涂膜进行了表征。结果表明：与传统乳液聚合得到的乳液及相应的涂膜相比,无皂乳液的耐电解质性能和涂膜的耐水性都有一定的提高,含氟单体有效地参与了聚合,涂膜的疏水性大大增强,耐热性显著提高。     

脂肪胺生产和应用的一些新进展

本文介绍最近三年来脂肪胺生产和应用的某些进展。主要包括：用作洗涤剂活性物的新型非离子物－脂肪胺聚氧乙烯醚的应用研究以及脂肪醇一步法制长链叔胺新型催化剂的研究和应用。文中还简单介绍了脂肪胺工业应用的途径。