【作者】 杨莹；

【导师】 夏清；

【作者基本信息】 天津大学 ， 化学工程， 2013， 硕士

【摘要】 4,4’-二氨基二苯乙烯-2,2’-二磺酸(DSD酸)作为生产荧光增白剂和染料的重要中间体，由于其良好的环保性能而得到广泛应用，在全球的需求量持续增长。同时，DSD酸生产工艺的中间产物，NTS酸，DNS酸等也是生产其他染料的中间体，因此，深入的研究DSD酸生产工艺的每个环节和各种中间产物具有很重要的实际意义。本文针对DSD酸生产中新的磺化，中和和氧化工艺，通过相关物系溶解度的测定，确定了工艺的可行性及关键点的工艺参数，为新工艺的实施提供了基础数据。本文首先测定了NTS和NTSNa在硫酸-水溶液中的溶解度，结果表明，NTS和NTSNa在硫酸-水溶液中的溶解度均随着温度升高而增大；随溶液中硫酸浓度的增加，NTS和NTSNa的溶解度先减小后增大，在硫酸质量分数为60%的硫酸-水溶液中溶解度最小；硫酸浓度小于30%时，NTS的溶解度大于NTSNa，且两者的差异随硫酸浓度增加而减小；硫酸浓度大于30%时，NTS和NTSNa的溶解度几乎相等。根据上述测定结果，确定了磺化反应后分离NTS的最佳条件及新的磺化、中和和氧化工艺的适宜操作范围；其次，测定了低硫酸浓度范围内NTSNa在NTS-硫酸-水三元溶剂中的溶解度，考察NTS的存在对NTSNa溶解度的影响，根据测得的溶解度数据，设计计算出新的磺化、中和和氧化工艺中关键流股的参数值；采用Apelblat经验方程关联溶解度数据，温度的均方根偏差在0.24~1.96K之间。根据已得的溶解度数据，结合该优化工艺中流股关系，经过分析和计算，得到具体操作参数的理论值，通过实验验证，表明适当调整理论值，即可实现操作，达到预期的目标，因此本文实现了该磺化和氧化工艺的优化。更多还原

【Abstract】 As the important intermediate of producing dyes and fluorescent brighteners,4,4’-diaminostilbene-2,2’-disulfonic acid(DSD acid) undergoes wide application andan increasing demand all around the world because of its environmental friendlycharacter. Meanwhile, the intermediates produced in the production of DSD are alsoimportant intermediates for dyes. Thus, further research of the steps and intermediatesin the production of DSD acid is meaningful in practice. This article aimed at the newoptimizing process of sulfonation, neutralization and oxidation steps in the productionof DSD. We determined the feasibility of the new process and the parameters of mainpoints by determining the solubilities of related systems, and provided the basic datafor the implement of the new process.First, solubilities of NTS and NTSNa in H2SO4-H2O system was determined, theresult shows that solubilities of the two substances both increase with the increase oftemperature; with the increase of the content of H2SO4, solubilities of NTS andNTSNa decrease at first and increase later, reach the lowest value when the massfraction of sulfuric acid is60%; when the mass fraction of sulfuric acid is less than30%, the solubility of NTS is bigger that that of NTSNa, the discrepancy goes downwith the increase of the content of H2SO4; when the mass fraction of sulfuric acid isbigger than30%, solubilities of NTS and NTSNa are almost equal. According to thedetermination result, we decided the best condition for the separating out of NTS aftersulfonation and appropriate operation range of the new process. Second, thesolubilities of NTSNa in the NTS-H2SO4-H2O system were determined, the influenceof the existence of NTS to the solubility of NTSNa was analyzed. According toobtained data, the paramaters of the key streams in the new sulfonation, neutralizationand oxidation process were designed and calculated. We used the modified Apelblatmodel to correlate the data. The root-mean-square deviation of temperature wasbetween0.24~1.96K.According to the obtained solubilities data, combining the relationship ofmaterial flows in the optimizing process, we got the theoretical values of the specificoperation parameters by analysis and calculation. After that, testing the values byexperiments, we found they were available and effective after appropriate adjustment. This work realized the optimizing process of sulfonation and oxidation step.更多还原