一种季铵盐阳离子表面活性剂的合成与性质

以氯丙烯与N,N-二甲基十二烷基胺(DTA)为原料合成了季铵盐阳离子表面活性剂十二烷基二甲基烯丙基氯化铵(DADAC);研究了原料配比、反应温度、反应时间和溶剂等因素对生成物DADAC收率的影响,通过红外光谱、元素分析确定其化学结构。较佳反应条件为:n(氯丙烯)∶n(DTA)=3∶1,无水乙醇为溶剂,50℃下反应24 h,DADAC收率为93.76%。最后测定了产物的表面性能,得到25℃下,DADAC的cmc为5.76 mmol/L,在cmc时的γ=34.2 mN/m,Krafft点<0℃。     

分光光度法测定水中微量阳离子表面活性剂

在pH=12.8的NaOH缓冲溶液中,显色剂2,6-二溴-4-硝基苯基重氮氨基-4-苯基-2-噻唑(DBNPDAPT)与阳离子表面活性剂十六烷基氯化吡啶(CPC)或十六烷基溴化吡啶(CPB)反应形成蓝紫色离子缔合物,基于此建立了一种分光光度法测定水中微量阳离子表面活性剂的方法。实验结果表明,缔合物的最大吸收波长为635 nm,表观摩尔吸光系数分别为2.30×104和1.73×104L·mol-1·cm-1,CPC和CPB的浓度在0～1.5×10-5mol·L-1范围内服从比尔定律。该方法应用于生活污水中微量阳离子表面活性剂(以CPC计)的测定,结果满意。     

阳离子表面活性剂与LAS的复配性能研究

采用新开发的带有乙氧基链的含氮阳离子表面活性剂———十二烷基二甲基羟乙基氯化铵(K3)与LAS进行复配,考察了复配体系的物化性能,如:界面张力、乳化力、润湿力、去污力以及K3对大肠肝菌、金黄色葡萄球菌的杀菌性能等。实验证明K3与阴离子表面活性剂有良好的复配性能与杀菌性能,对洗涤剂配方的改进,产品性能的提高具有指导意义。     

Gimini阳离子表面活性剂增敏光度法测定水中的微量Fe(Ⅱ)

在醋酸钠(NaAc)缓冲溶液存在下,以1-(2-吡啶偶氮)-2-萘酚(PAN)做显色剂,Gimini阳离子表面活性剂对PAN与Fe(Ⅱ)显色反应具有增敏作用。结果表明,最大吸收波长为536nm处,pH为5.6时,表面活性剂用量1.0mL,显色剂用量0.8～1.0mL,显色时间为15min时,Fe(Ⅱ)-PAN-Gemini14三元络合体系能形成稳定的红色配合物,用一元线性回归法求得该体系表观摩尔吸光系数为1.8×105L/(mol·cm),并用该三元络合体系测得玄武湖水样中铁的含量为1.0μg/mL。     

分光光度法测定阳离子表面活性剂在砂岩表面的吸附

为测定阳离子表面活性剂十六烷基三甲基氯化铵(1631)在岩石表面的吸附量,利用紫外分光光度法,检测了1631溶液在岩石表面吸附前后的质量浓度,算出1631在岩石表面的吸附量。结果表明,用紫外分光光度法检测阳离子表面活性剂浓度快速准确,确定617nm为测定波长,线性回归方程为y=0 0027x-0 0058,R2=0 9991;不同砂岩表面的吸附平衡时间不同,亲水表面为10h,油表面为16h,砂表面为18h;同砂岩表面的静态饱和吸附量不同,亲水表面是0 7mg·g-1·砂,亲油表面是1 4mg·g-1·砂,油砂表面是6 7mg·g-1·砂;天然岩心动态吸附量为0 8066mg·g-1·砂。     

十二烷基多季铵盐Gemini型阳离子表面活性剂合成

控制反应物乙二胺与环氧氯丙烷的配比，得到乙二胺与环氧氯丙烷的摩尔比分别为1：5、1：4、1：1的产物。然后与自制十二烷基二甲胺进一步反应温度60℃；反应时间1h：反应溶剂、水和乙醇的混合溶剂。通过测定不同浓度下溶液的表面张力，得到其产物I、Ⅱ的临界胶束浓度为0.05%（质量百分比）左右。说明产品具有很低的临界胶束浓度和较好的表面活性。进一步的实验证明；合成产物具有较好的发泡力、稳泡力和金属腐蚀的抑制性能，并考察了其与阴离子表面活性剂的复配性能。     

1227两种测定方法的对比和分析

通过实验对测定十二烷基二甲基苄基氯化铵活性物含量的两种方法进行了比较和分析。结果表明,两种测定方法无显著性差异,都适用于检测常规产品。其中四苯硼钠滴定法(HG/T 2230—2006))由于液相容易有结块挂壁现象,使测定值偏低,受温度影响变化大,不适于检测高含量加防冻剂的产品,但其精密度较好。四苯硼钠两相滴定法(QB 1915—1913)抗干扰能力强,适用范围广,但要注意观察终点的判断。     

利用新叠氮试剂（PTBAS）分光光度法测定阳离子表面活性剂CTMAB

提出了一种用新叠氮试剂３－（苯偶氮苯）－１－三氮烯苯甲酸钠与阳离子表面活性剂溴化十六烷基三甲铵形成离子缔合物而测定ＣＴＭＡＢ含量的新方法。该法具有很好的灵敏度和选择性，是一种很有应用前景的９测定ＣＴＭＡＢ的新方法。     

新型Gemini阳离子表面活性剂的合成及其性能研究

在中性或弱酸性水溶液中,二乙胺和环氧氯丙烷反应生成季铵盐中间体,再与十二烷基二甲基胺反应制备了新型多烷基多季铵盐Gemini型阳离子表面活性剂.其临界胶团浓度(CMC)为4×10-6 mol·L-1、克拉夫点(Krafft point)＜0℃.     

关于阳离子表面活性剂水溶液表面张力的测定

本文自实验结果说明,阳离子表面活性剂水溶液表面张力的测定应当采用适当的方法,否则将得出不正确的表面张力数据,从而得到错误的有关阳离表面活性剂表面活性的结论。     

复合肥中缩二脲测定方法的改进

对GB/T 22924—2008复合肥中缩二脲的测定方法 (分光光度法)中的试样处理步骤进行改进,即采用直接定容后过滤代替多次洗涤收集滤液,同时将显色体积从50 mL改为100 mL。改进后测定步骤简化,分析时间缩短1 h,加标回收率为97.2%~103.3%,方法准确可靠。     

Pyrimidinium cationic surfactants as emulsifiers for oil-in-water emulsions

Pyrimidinium cationic surfactants with 13–17 carbon atoms in the hydrophobe were used as emulsifiers for oil-inwater (heptane/water) emulsions at concentrations near the critical micelle concentrations. Interfacial tensions of the emulsifier solutions in water against heptane were measured. Drop size distributions of the emulsions were determined at different times using microscopic techniques, and the rate of coalescence was calculated. The structure having 16 carbon atoms in the alkyl chain had coalescence rates lower than the other structures, including two conventional C-16 cationics used as controls.     

Primary aerobic biodegradation of cationic and amphoteric surfactants

The primary aerobic biodegradation of several cationic and amphoteric surfactants has been studied by using the shaking-flask degradation test and orange II spectrophotometric analysis. The results show that cationic and amphoteric surfactants can be readily biodegraded, with their degradation exceeding 94%. The degradation kinetics can be accurately described by the Boltzmann model. The relationship between structure and biodegradability is discussed. The presence of hydrophobic groups has a strong effect on the biodegradability of these surfactants. Biodegradability decreases with increasing chain length. The presence of hydrophilic groups mainly affects the degradation rate of these surfactants, but not their ultimate biodegradeability. Bio-degradability is deterred and degradation is slowed as steric hindrance increases. Degradation rates increase markedly when hydrophilic groups containing an amide bond are pres-ent.     

Kinetics of precipitation of surfactants. I. Anionic surfactants with calcium and with cationic surfactants

Isoperibol calorimetry was used to measure the rates of precipitation for aqueous solutions of several anionic surfactants with calcium and of anionic and cationic surfactants. A monomer concentration-dependent supersaturation ratio was used to describe the relative rates of precipitation for the surfactant systems studied. This supersaturation ratio allows for the relative rates of precipitation of any surfactant solution to be compared whether micelles are present in solution or not. In general, as the supersaturation ratio increases, the rate of precipitation decreases and the induction time decreases, bot above and below the critical micelle concentration (CMC). The rate of precipitation of sodium dodecyl sulfate (SDS) with dodecyl pyridinium chloride is much slower than the rate of precipitation of the anionic surfactants with calcium for similar supersaturation ratios. The rate of precipitation of SDS with calcium is slightly faster than the rate of precipitation of sodium octyl benzene sulfonate for similar supersaturation ratios. Studies of precipitate crystals, conducted using image analysis, showed that size and shape dependent on the initial supersaturation, the precipitating surfactant molecule, and the extent of aging (until an equilibrium size and shape was reached). Also, differences in the appearance of crystals formed from solutions above and below the CMC were observed. These were most likely due to the difference in supersaturation of these solutions. The crystals formed due to precipitation of SDS with calcium at a concentration above the CMC formed flat trapezoidal, rhombic and hexagonal shapes. These aged into clusters by 1 wk. For a solution that was precipitated at concentrations beginning below the CMC, the crystals began as elongated and rhombic flat plates and aged into trapezoidal, rhombic, and needle-like structures.     

酯型双子阳离子表面活性剂与甲基橙的相互作用

通过紫外-可见光谱法研究了一系列具有不同疏水基的、含酯基双子季铵盐阳离子表面活性剂(EDC-1,2,3,4)与甲基橙(MO)之间的相互作用.结果表明,表面活性剂浓度在1.0×10-5 mol·L-1左右时(远低于其cmc),EDC和MO聚集.这种聚集导致MO的紫外吸收光谱中π→π*吸收带蓝移98 nm,即在365 nm处形成一个新的吸收带.进一步增加EDC浓度至cmc以上时,由于MO增溶于EDC胶束内部,使λmax移至430 nm处.并且分离出了EDC与MO聚集产生的聚合物,经1HNMR分析,其中EDC与MO的摩尔比为12.     

含酯基双子季铵盐阳离子表面活性剂的合成及性能

分别以氯乙酸辛酯 ,氯乙酸十二醇酯、氯乙酸十四醇酯和四甲基乙二胺反应合成了相应的含酯基双子季铵盐阳离子表面活性剂化合物 (Ⅰ～Ⅲ )。滴体积法测定化合物Ⅰ～Ⅲ的表面张力和cmc。γcmc分别为2 7 3 1、 3 3 73和 3 4 0 1(mN/m) ,cmc分别为 5 0 1× 10 -3 、 3 98× 10 -3 和 3 16× 10 -3 (mol/dm3 )。     

生物可降解型阳离子酯类表面活性剂的研究

以自制的失水甘油基三甲基氯化铵(GTMAC)和硬脂酸为原料,经一步反应合成阳离子单酯表面活性剂(CMESA)。研究了反应介质、反应温度和反应时间对生成物CMESA收率的影响,通过元素分析、官能团分析和红外光谱确证其化学结构,较佳反应条件为:n(GTMAC)∶n(硬脂酸)=1∶1,异丙醇为溶剂,85℃,反应16h,CMESA收率86 8%。接着采用电导法测临界胶团浓度(cmc),拉环法测表面张力(γ),得到20℃下CMESAcmc为0 035mmol/L,在cmc时的γ=44 95mN·m-1。最后研究了在静态时厌氧污泥对CMESA的作用,结果表明:厌氧污泥对CMESA适应性强,其产甲烷气的量不受影响,IC50可能超过1 0g/L。     

聚氧乙烯醚类表面活性剂生物降解度测定方法的改进

对聚氧乙烯醚类非离子表面活性剂生物降解度的测定方法———硫氰酸钴法进行了改进:三氯甲烷取代苯作为萃取剂;萃取次数从1次增加到3次;硫氰酸钴与表面活性剂的络合反应时间为15 min。实验结果表明:重复性实验的相对标准偏差<6.0%;对AEO7、Tween85和AEO30的平均回收率在97%~104%,相对标准偏差<4.0%。对原方法不宜测定的一些类型的聚氧乙烯醚类非离子表面活性剂的生物降解度进行测定,结果表明:对单EO链、单烷基链非离子表面活性剂,EO数从3~12可扩大到3~30,并能测定多个EO链、多个烷基链聚氧乙烯醚类非离子表面活性剂的生物降解度。     

Flotation of perrhenates with cationic surfactants: Effect of surfactant's structure

An experimental investigation is presented on the flotation of perrhenate anions from diluted aqueous solutions (5.10^?5 M ) with numerous cationic surfactants of systematically varying molecular structure. Alkyltrimethyl-ammonium bromides, alkoxycarbonylmethyl-trimethylammonium chlorides, alkoxycarbonylmethyl-dimethylbenzylammonium chlorides, ethoxycarbonylmethyl-dimethylalkylammonium chlorides, N-substituted dodecylamines, and diquaternary ammonium bromides were investigated at their initial concentrations in the feed solution, 1.10^?4 M or 2.10^?4 M . It was found that both the length of the main hydrocarbon chain and of the short hydrocarbon groups govern the affinity of a cationic surfactant towards perrhenate anions. In order to achieve the effective flotation of perrhenate or similar anions the value of C:N atomic ratio for a tertiary or a quaternary ammonium surfactant should be in the range 15 to about 26. This value can be used as a primary criterion for the sufficient flotation capability of an alkylammonium surfactant.     

水中阴离子表面活性剂测定方法概述

简要介绍了表面活性剂的性质,阴离子表面活性剂的种类及其对水体环境的危害;重点对水中阴离子表面活性剂的测定方法即分光光度法、两相滴定法、高效液相色谱法、薄层层析法及离子选择性电极分析法等进行了综述;提出了水中阴离子表面活性剂测定方法向信息化、实时快速在线监测智能化和检测仪器向微型化的方向发展。