双十八烷基四羟乙基二溴丙二铵的微波合成及其性能研究

以十八烷基二乙醇胺、1,3-二溴丙烷为主要原料,在微波高压条件下进行季铵化反应合成了一种双子表面活性剂双十八烷基四羟乙基二溴丙二铵(DTDD),通过红外光谱(IR)和核磁共振(~1H NMR)对DTDD进行了表征,并用液相色谱-质谱联用(LC-MS)测定了其纯度。通过单因素、正交实验得到了微波法合成目标产物的最佳合成条件为:设置微波功率为900 W,反应时间8 h,反应温度为140℃,产品收率达92%以上。与传统加热法对比,使用微波合成法反应速率大大提高。性能测试结果表明:对比单链季铵盐(OMDAB),目标产物DTDD具有良好的表面性能,其临界胶束浓度为0.087 g/L,相应的表面张力γ_(CMC)为31.09 mN/m。     

双十八烷基二羟乙基溴化铵的微波合成及性能

以十八烷基二乙醇胺和溴代十八烷通过微波合成技术制备了双十八烷基二羟基溴化铵季铵盐（DODAB）。确定最佳合成工艺条件为：反应物浓度为2.17 mol·L^-1、反应时间为158.61 min、微波功率为626.06 W，在此条件下转化率的预测值为93.71%。产品由IR和¹H NMR进行表征。测定产品的表面活性为：CMC=0.501 g·L^-1，表面张力为30.27 mN·m^-1，优于阳离子表面活性剂D1821。测定产品应用于织物的柔软性能，结果显示：DODAB的柔软效果与D1821相当，随着处理的次数增多，DODAB处理后的柔软效果虽比D1821稍微弱一些，但其手感上会更为自然，更为舒适。同时，DODAB较D1821有着更好的维持织物白度性能的效果，具有较好的抗黄变能力。     

烟酸类表面活性剂的合成研究

以烟酸为原料,通过卤置换反应、酰胺化反应、季铵化3步反应,合成[3,3'-(对苯二氨甲酰基)]双N-烷基吡啶溴盐表面活性剂目标产物。用IR、1HNMR、13CNMR和MS对目标产物进行确认和表征,并通过单因素试验,确定了较佳的合成条件:n(双(烟酰基)对苯二胺)∶n(溴代烷)=1∶2.6,反应温度140℃,反应时间6 h。利用紫外分光光度法测量目标产物的临界反胶团浓度CrMC分别为2.09×10-5、2.27×10-5和2.39×10-5mol/L。     

山嵛酸双酯基有机硅季铵盐的微波合成工艺及性能

以山嵛酸、N-甲基二乙醇胺以及γ-氯丙基三甲氧基硅烷为主要原料,分别经过酯化和季铵化反应两步合成了一种超长碳链的双酯基有机硅季铵盐,并通过单因素、正交试验得到了微波法合成目标产物的最优工艺条件为：设置微波功率为800W,物料摩尔比为n（硅烷）∶n（酯胺）=1.2∶1,反应温度为170℃,溶剂用量为m（溶剂）∶m（原料）=0.8∶1,反应时间为12h,产品产率达96.60%。此方法克服了长链叔胺季铵化过程中普遍耗时过长的困难,提高了反应速率,而且实验重复性良好。实验中采用红外光谱、核磁共振氢谱对中间体及目标产物的结构进行了表征,与预期结果一致;建立了高效液相色谱-蒸发光散射检测器（HPLC-ELSD）测定季铵盐纯度的方法,基线稳定,峰型良好,产品纯度达98.77%,具有一定的参考价值。性能测试结果表明：对比DC-5700,目标产物具有良好的热稳定性,优异的乳化及增溶性能;其水溶液的临界胶束浓度为1.81mmol/L,表面张力（γ_CMC）为49.4mN/m。     

酰胺键为间隔基的吡啶双子表面活性剂合成及性能

以乙二胺、1-溴代烷、氯乙酰氯和吡啶为原料,经卤代、酰胺化和季铵化反应合成了系列酰胺键为间隔基的吡啶双子表面活性剂。目标产物合成条件:超声波(40kHz,100W)辅助反应,反应温度60℃,反应时间5h。用 FTIR、¹H NMR、¹³C NMR对目标产物进行了结构表征,对目标产物的临界胶束浓度(cmc)、乳化性、泡沫稳定性和杀菌性能进行了考察。实验结果表明,该系列产物的临界胶束浓度cmc 为1.4×10^-2～2.3×10^-5mol/L,具有较好的乳化性和稳泡性。在浓度为100mg/L时,烷基链碳原子数为8的表面活性剂对大肠杆菌和枯草芽孢杆菌的抑菌效果最好。     

南京大学研发出新型双子型氟碳表面活性剂

南京工业大学开发了一种新型双子型氟碳表面活性剂，已取得专利。该表面活性剂是以亲水性的单酯二氯丙烷为联接基团的新型亲水柔性间隔基的双子型氟碳表面活性剂。该表面活性剂通过全氟烷基磺酰氟与N，N-二甲基-1，2-乙二胺或N，N-二甲基-1，3-丙二胺反应得中间产物N-[（二甲氨基）-烷基）全氟烷基磺酰胺，然后与单酯二氯丙烷进行季铵化反应而得产品。该表面活性剂能极大降低溶液的表面张力，起泡力强，去污力优良且无异味，色泽佳，复配性能好，合成工艺简单。     

新型喹啉Gemini表面活性剂的合成及界面吸附

以6-氨基喹啉，三光气，三乙胺为原料合成了对称的喹啉脲，通过其与三种溴代烷进行季铵化反应合成了喹啉双季铵盐，其结构经FT-IR，1H NMR，13CNMR和ESI-MS证实。对中间体喹啉脲及目标产物喹啉Gemini表面活性剂的合成条件进行了优化。合成中间体的反应条件为二氯甲烷做反应溶剂，n (6-氨基喹啉)∶n (三光气) = 5∶1，反应时间为6 h，收率可达88%。合成喹啉类Gemini表面活性剂的反应条件为DMF为反应溶剂，反应温度为110℃，n(中间体)∶n(溴代烷) = 1∶14，反应时间为8 h，收率可达74%。对目标产物喹啉Gemini表面活性剂在三氯甲烷-水体系中的界面张力进行了测定，结果表明：喹啉Gemini表面活性剂在三氯甲烷溶液内扩散到三氯甲烷-水界面是由纯扩散吸附控制的。     

一种可聚合双季铵盐表面活性剂的合成与表征

以N,N-二甲基十二烷基叔胺盐酸盐、环氧氯丙烷为原料合成了中间产物N-3 -氯-2-羟丙基-N,N-二甲基十二烷基氯化铵.中间产物再和N-乙烯基咪唑(Ⅵ)发生季铵化反应,合成了一种可聚合双季铵盐表面活性剂,研究了原料配比、反应温度和反应时间对目标产物乙烯基咪唑双季铵盐产率的影响.结果表明,较佳工艺条件为:n(Ⅵ):n(中间产物)=1.2∶1,反应温度为80℃,反应时间为12 h,在此条件下,目标产物的产率达到81.2％.并利用IR,MS和1HNMR对产物结构进行了表征.     

含咪唑啉环不对称双季铵盐的合成及其缓蚀性能

以长链烷基叔胺、长链烷基叔胺盐酸盐、环氧氯丙烷为原料合成了N-(3-氯-2-羟丙基)-N,N-二甲基长链烷基季铵盐,利用其与长链烷基咪唑啉季铵化合成了含咪唑啉环的不对称双季铵盐。通过FTIR,1HNMR验证了中间体和目标产物结构,考察了其合成工艺。合成含咪唑啉环不对称双季铵盐的最佳反应条件为:n[N-(3-氯-2-羟丙基)-N,N-二甲基长链烷基季铵盐]∶n(长链烷基咪唑啉)=1∶1.1,反应溶剂采用异丙醇,反应温度80℃。用失重法测定了25℃时含咪唑啉环不对称双季铵盐在1.0mol/L盐酸溶液中的缓蚀性能,结果表明,仅添加50mg/L,对Q235钢缓蚀率达98.89%。     

m-n-m型Gemini季铵盐表面活性剂的合成及性能研究

以N,N-二甲基十四胺和1,8-二溴辛烷反应生成了14-8-14型Gemini季铵盐表面活性剂,通过单因素试验优化了反应条件,确定较佳合成条件为:N,N-二甲基胺的用量为5 mmol,N,N-二甲基胺与二溴烷烃的摩尔比为2.2:1,溶剂乙腈用量为10 mL,反应温度为80℃,反应时间为24 h,在此条件下合成了24种m-n-m型Gemini季铵盐表面活性剂,大部分反应的收率大于80%。采用吊环法对产物的表面张力进行了测定,分别研究了疏水烷基链、连接基对Gemini季铵盐表面活性剂表面活性的影响,研究发现,当连接基n相同时,随着疏水烷基链的增长(m10时),Gemini季铵盐表面活性剂的表面张力呈现先减小后增大的趋势,14-n-14型Gemini季铵盐表面活性剂呈现出最好的表面活性;当疏水烷基链m=14时,随着连接基n的增大,Gemini季铵盐表面活性剂的表面张力呈现先增大后减小的趋势。     

棕榈酰基蛋氨酸表面活性剂的合成与性能

以天然产物棕榈酸和蛋氨酸为原料，通过酰氯化反应和酰胺化反应两步法合成棕榈酰基蛋氨酸表面活性剂（PMS），探究反应温度、反应时间、反应物摩尔比、反应介质体积比等因素对酰胺化反应的影响；通过傅里叶红外光谱（FTIR）、核磁共振氢谱（¹H NMR）和质谱对产物的结构进行表征；研究产物的表面性能和复配体系的性能。实验结果表明：酰胺化反应最佳反应温度为30℃、n(棕榈酰氯)∶n(蛋氨酸)=1∶1.2、V(水)∶V(丙酮)=1∶2、反应时间为2.5h，在此条件下，得到产物产率89.0%；表征的结果为目标产物；合成产物临界胶束浓度为 1.2×10^-4mol/L，表面张力为29.59mN/m；对苯等有机溶剂的乳化作用明显优于月桂酰基谷氨酸（LAS）；PMS与椰油丙基甜菜碱（CPBS）摩尔比为4∶6时复配体系表面活性最佳，临界胶束浓度达到9.5×10^-5mol/L，复配体系表面张力为28.1mN/m。     

A New Anionic Oxalamide Lauryl Succinate Sodium Sulfonate Gemini Surfactant: Microwave-Assisted Synthesis and Surface Activities

An anionic Gemini surfactant, oxalamide lauryl succinate sodium sulfonate, was synthesized successfully through amidation, esterification and sulfonation reactions under microwave irradiation conditions by using maleic anhydride, ethylenediamine, lauryl alcohol, sodium sulfite as the starting materials. The best reaction conditions for synthesize the target product were obtained by single factor and orthogonal optimization methods. FTIR, elemental analysis and ¹H‐NMR analysis were used to confirm the chemical structure of the surfactant. The critical micelle concentration (CMC) in aqueous solution, surface tension, emulsification capacity and foaming power were determined. The critical micelle concentration and γ_CMC are respectively equal to 3.5 × 10^?4 mol L^?1 and 21.5 mN m^?1. It was found that microwave‐assisted synthesis is an efficient means of preparation of this anionic Gemini surfactant with shorter times and higher yields.     

油酸酰胺基二苯醚双磺酸钠的合成及表面活性测定

以对硝基二苯醚、油酸酰氯、氯磺酸为主要原料,通过硝基还原反应、胺基酰化反应、磺化反应,合成了双子表面活性剂油酸酰胺基二苯醚双磺酸钠;并用IR,1HNMR,MS对产品及中间体结构进行了表征。测定了其水溶液表面活性和临界胶束浓度(CMC),结果表明,其CMC(2 14mmol/L)低于传统的单疏水基单亲水基型表面活性剂十二烷基苯磺酸钠(SDBS),并具有较高的活性,其水溶液表面张力可降至34 0mN/m。     

硫酸酯盐双子表面活性剂的合成和界面张力的研究

实验室条件下,以长链羧酸(月桂酸)、聚乙二醇等为主要原料,通过赫尔-乌尔哈-泽林斯基反应等和酯化反应,用醚键加入方式加入联接基团,用浓硫酸加成反应加入硫酸酯键,从而在实验室条件下合成具有特殊结构的双子表面活性剂-GA12-S-12.通过用旋转液滴法测合成的硫酸酯盐阴离子双子表面活性剂的表面张力,测得其临界胶束浓度(CMC)为438 mg/L,临界胶束浓度下表面张力为30.9 mN/m,并对比十二烷基硫酸钠水溶液表面张力,显示GA12-S-12[低聚二醇(α-硫酸酯钠)月桂酸双酯阴离子双子表面活性剂]具有更优的表面活性.进一步配制不同浓度的GA12-S-12表面活性剂溶液,测定它们与长庆五里湾原油的界面张力,效果显示其适用于五里湾区原油采收率的提高.     

Physicochemical Properties of Novel Phosphobetaine Zwitterionic Surfactants and Mixed Systems with an Anionic Surfactant

A series of novel zwitterionic phosphobetaine (PPBT) surfactants were synthesized using long chain fatty alcohol, epichlorohydrin, dimethylamine and sodium dihydrogen phosphate as raw materials. The physicochemical properties of the phosphobetaine surfactants such as isoelectric point, foaming, surface tension, critical micelle concentration (CMC) and Krafft point were measured. Low CMC and surface tension values indicated the surface activities of the phosphobetaine surfactants were quite excellent. The CMC and surface tension values of PPBT/SDS mixed systems were determined. It was found both of CMC and surface tension values decreased compared with single surfactant system because of the association between dodecyl sulfate anions and cationic groups in phosphobetaine by electrostatic attraction.     

Synthesis and Micellization Properties of New Anionic Reactive Surfactants Based on Hydrogenated Cardanol

We report the synthesis, characterization and micellization properties of two anionic reactive surfactants based on 3-pentadecyl phenol obtainable from a renewable resource, cardanol. The synthesis is achieved through simple chemical transformations, first converting the phenol to the acrylate that is sulfonated in a second step. The products were characterized by elemental analysis and spectroscopic techniques. The surfactant properties of the sulfonated acrylates were measured and compared with the standard non-reactive anionic surfactant sodium dodecyl sulfonate. The micellization behavior of aqueous solutions was studied using conductivity, surface tension measurements, and the fluorescence probe technique based on diphenyl hexatriene. Characterization by surface tension measurements facilitated the determination of basic surfactant properties like the critical micelle concentration (CMC), the surface tension at the CMC, surface excess and area per surfactant molecule. The Gibbs free energy of micellization showed a negative value suggesting spontaneous micellization in aqueous solution. The micellization of the surfmer with an ethylene spacer between the phenyl ring and the acrylate group seems to be enhanced as indicated by the lower surface excess and lower free energy. Its CMC was also lower.     

Synthesis, Characterization and Surface Activity of Alkyl m-Xylene Sulfonate Isomers

This paper deals with the synthesis of a series of alkyl m-xylene sulfonate isomers (with the m-xylene located at the eighth carbon atom along the long alkyl chain) by the Friedel?CCrafts reaction, and the Grignard reaction followed by hydrogenation. The structures were confirmed by ¹H NMR. All analytical methods indicated high levels of purity of the isomers with the eighth carbon atom at the long alkyl chain. The critical micelle concentration (CMC), surface tension and maximum surface excess concentration at the CMC and area per molecule at the interface were determined. As the long alkyl chains increased the surfactant molecule tends to pack closely at the gas?Cliquid interface. Accordingly, the CMC decreased, the adsorption density increased, and the surface tension reduction was strengthened.     

含多官能团Gemini表面活性剂的合成及性能

以氯乙酰氯、间苯二甲酰氯、长链伯胺（碳链长度为8、12、14和16）和N,N-二甲基乙醇胺为原料合成了一系列含多官能团Gemini阳离子表面活性剂目标产物（I₈、I₁₂、I₁₄和I₁₆）。采用红外光谱和核磁氢谱对产物进行了结构表征。通过电导率法测量目标产物在不同温度下的临界胶束浓度（CMC），并计算出胶束的热力学参数（、、）；在298.15K条件下，通过表面张力法测定目标产物的表面张力（γ_CMC），并探讨了目标产物的泡沫性能和乳化性能。结果表明：目标产物有较低的临界胶束浓度值（CMC），在298.15K条件下，最低CMC达到0.05mmol/L；I₁₆的γ_CMC最低为36.14mN/m；泡沫性和乳化性测试结果表明，在298.15K条件下，I₈的起泡能力最好，I₁₂和I₁₄的稳泡性最好，均达到100%；目标产物对苯和二甲苯具有很好的乳化性能，其中I₁₂对二甲苯的乳化性能最好，乳化时间为900s，I₁₆对苯的乳化性能最好，乳化时间为629s。     

A Star-Shaped Anionic Surfactant: Synthesis,Alkalinity Resistance,Interfacial Tension and Emulsification Properties at the Crude Oil–Water Interface

In this research, a star‐shaped surfactant was synthesized through the chlorination reaction, alkylation reaction and sulfonation reaction of triethanolamine, which is composed of three hydrophobic chains and three sulfonate hydrophilic groups. The critical micelle concentration (CMC) of the surfactant was measured by the surface tension method, and the results showed that it had high surface activity with CMC of 5.53 × 10^?5 mol/L. The surfactant was superior in surface active properties to the reference surfactants SDBS and DADS‐C₁₂. The interfacial tension (IFT) of the studied crude oil–water system (surfactant concentration 0.1 g/L, NaOH concentration 0.5 g/L, and experimental temperature 50 °C) dropped to 1.1 × 10^?4 mN/m, which can fulfil the requirement of surfactants for oil displacement. An aqueous solution of the surfactant and crude oil was emulsified by shaking, which formed a highly stable oil‐in‐water (O/W) emulsion with particle size of 5–20 μm. The oil displacement effect was almost 12%.