新型阳离子表面活性剂十二烷基甲基二羟乙基溴化铵的合成与性能研究

【作者】 毛桃嫣；

【导师】 郑成；

【作者基本信息】 广州大学 ， 化学工艺， 2010， 硕士

【摘要】 本论文以N-甲基二乙醇胺与溴代十二烷为原料,分别采用了微波和无溶剂合成的方法,合成了新型的表面活性剂十二烷基甲基二羟乙基溴化铵(DBMAC)。经IR和1H NMR分析鉴定了产物的结构。通过响应面分析法(RSM)建立了反应转化率与各因素之间的数学关系模型,对微波合成十二烷基甲基二羟乙基溴化铵的工艺进行了优化;确定了最佳反应条件为:溶剂体积为6.90mL,微波功率为636W,反应时间为23min,转化率为92.18%。该法与传统方法相比,合成时间仅为传统方法的5.48%。无溶剂合成十二烷基甲基二羟乙基溴化铵的最佳反应条件为:温度90℃,反应时间为150min,反应物的摩尔比为1:1,转速为200 r·min-1,转化率为90.2%。将产品进行放大研究,提出了影响放大合成过程和产率的温度梯度及浓度梯度、反应周期等因素的解决方案。对产物的表面性能和应用性能进行测试研究,得到其表面张力为24.2N·m-1,临界胶束浓度为1.67×10-4mol·L-1,克拉夫点小于0℃,熔点为111.2-111.9℃;其增溶性能、再润湿力很好,有一定的乳化性能、发泡力和柔软性能,以及其对织物白度的影响较小。同时对表面活性剂十二烷基甲基二羟乙基溴化铵的合成,分别在微波作用以及传统加热两种方式下,通过在不同的沸腾温度下反应,获得微波合成反应的动力学参数,分析微波作用。结果表明,微波的作用没有改变反应级数,两种情况下都是一级反应。微波作用下的活化能为Ea=41.44kJ /mol;而传统加热的活化能为Ea =61.21 kJ /mol。本实验研究提出以单位时间单位容积内,微波作用下反应物的变化量减去相同温度条件下传统加热时的变化量,作为微波对反应速率的贡献量△(-rA )的概念。实验结果表明,在同一温度条件下,反应时间越短,即反应物浓度越高,微波对反应速率的贡献量△(-rA)就越大;在其它条件相同时,反应温度越低,微波对反应速率的贡献量△(-rA)就越大。更多还原

【Abstract】 A new type cationic surfucant– dodecyl methyl dihydroxyethyl ammonium bro- ide(DBMAC)was syhthesized from N-Methyldiethanolamine and bromododecane in this study. The structure of the product was characterized with IR and 1 H NMR.Through RSM, the mathematical relational model between conversion rate and factors was established, and the microwave synthesis technique of dodecyl methyl dihydroxyethyl ammonium Bromide was optimized. The results showed that the most suitable condition for the reaction were as follow as: solvent volume was 6.9 mL,the microwave irradiation power was 636 W,the radiation time was 23min,and the yield reached up to 92.18%.Compared with traditional method,the time of synthesis was only 5.48%.The most suitable condition for the synthesis of dihydroxyethylbenzylmethyl ammonium Bromide was optimized. The results showed as follow as: the temperature was 90℃,the radiation time was 150min,the mole ratio was 1:1, the rotate speed was 200 r·min-1,and the yield reached up to 90.2%. According to the best reaction conditions amplification experiment was made.The amplify of synihesis course was studied,The solvents of influence of temperature grads and concentration grads,and reaction periods etc.Through determination and study on the surface properties and application performance of DBMAC, the CMC was 1.67×10-4mol·L-1, surface tension was 24.2N·m-1, Krafft Point was below 0℃and melting point of the product was 111.2~111.9℃. At the same time, it showed good solubilization and deuto-wetting property of the surfactant. Its emulsification property, foaming power and softening property were also quite well; besides the effect on fabric whiteness was lower.The reaction were studied under microwave irradiation and conventional heating on the different boiling temperature point of the solvents. The kinetic parameters were obtained and analysis the effect of microwave.Results show that,the effect of microwave did not alter order of reaction. The activation energy is 41.44kJ /mol under microwave irradiation.while the actactivation energy is 61.21kJ /mol under normal heating. The new concep t of microwave devotion△(-rA) for chemical reaction was proposed in this paper. It is the increment of the reaction rate of microwave reaction and traditional reaction. The experimental result indicated that in the same temperature, the lower reactant concentration, the higher of the microwave devotionΔ(-rA). And the lower of temperature, the higher of the microwave devotionΔ( - rA ).更多还原