【作者】 王晓燕；

【导师】 吕早生；

【作者基本信息】 武汉科技大学 ， 化学工艺， 2005， 硕士

【摘要】 本论文在总结前人研究工作的基础上,采用亲核取代反应合成了磺酸乙酸钠。我们分别以氯乙酸和氯乙酸乙酯为原料,亚硫酸钠为磺化剂合成了目标产物。系统研究了反应温度、反应物摩尔比、溶剂配比及反应物浓度对转化率的影响; 运用正交实验确定了最佳反应条件,初步探讨了反应机理。以氯乙酸为原料时的最佳反应条件为:温度50℃,反应物摩尔比（Na₂SO₃/ClCH₂COOH）1.2:1,氯乙酸浓度1.2M,此时产率达53.42%; 以氯乙酸乙酯为原料时的最佳反应条件为:温度70℃,溶剂配比（水/乙醇的体积比）85:15,反应物摩尔比（Na₂SO₃/ClCH₂COOC₂H5）1.40:1,此时产率达50.23%。结果表明:以氯乙酸和氯乙酸乙酯为原料采用亲核取代反应合成磺酸乙酸钠是可行的。在反应过程中用电位分析法来测定反应液中的氯离子浓度,以此来判断反应进度,摧算产率,运用重结晶技术对产品进行分离提纯。利用傅立叶红外光谱、离子色谱、元素分析等提供的信息,对合成产物进行分析鉴定。分析鉴定结果表明:合成的产物为磺酸乙酸钠。最后,对合成的目标产物进行量子化学计算,得到了物质的能量、键长、键角和红外光谱等数据。通过比较可知这些计算结果和实验结果具有很好的一致性,这说明了计算所选用的HF、MP2方法是合理的。更多还原

【Abstract】 According to previous research work, the sulfoacetic acid disodium salt was synthesized by a nucleophilic substitution reaction in this paper. The target product was synthesized by using chloroacetic acid and ethyl chloroacetate as raw material and sulfite sodium as sulfonating agent. The effects of reaction temperature, reactant ratio, solvent ratio and reactant concentration on conversion were studied; we identified a good reaction condition by using orthogonal experiment and gave a preliminary analysis on the mechanism of reaction. When we use chloroacetic acid as raw material, the optimum reaction condition is: reaction temperature 50℃, reactant mole ratio 1.2:1, chloroacetic acid concentrate 1.2M, which give the yield of 53.42%; when we use ethyl chloroacetate as raw material, the optimum reaction condition is: reaction temperature 70℃, solvent ratio 85:15, reactant mole ratio1.40:1, which give the yield of 50.23%. The results show that the method which synthesize sulfoacetic acid disodium by using chloroacetic acid and ethyl chloroacetate as raw material and sulfite sodium as sulfonating agent by nucleophilic substitution reaction is feasible. In the course of reaction, the concentration of chlorine ion was identified by using electric potential analysis method, in order to estimate reaction degree and reckon the yield. The product was separated and purified by crystal method, the structure was validated by the information provided from FTIR, IC and element analysis. The results show that the product is sulfoacetic acid disodium salt. At last, we calculate the structure of the target product by quantum chemistry, we get the information of energy, bond length, bond angle and IR spectrum by this calculation. There is a good consistency between the calculated results and experimental results according to compare the results, which show the FH and MP2 methods are reasonable.更多还原