MDC热分解制备MDI的过程基础研究
文献类型：学位论文
| 作者 | 姚星星 |
| 学位类别 | 硕士 |
| 答辩日期 | 2010-05-25 |
| 授予单位 | 中国科学院研究生院 |
| 导师 | 李会泉 |
| 关键词 | 异氰酸酯 非光气 热分解 衍生法 动力学 |
| 其他题名 | Study of the process foundation of synthesizing MDI by the thermal decomposition of MDC |
| 学位专业 | 化学工艺 |
| 英文摘要 | Methylene-4,4’-di(phenylisocyanate) (MDI) is an important raw material and is manufactured by the phosgene route in the organic chemical industry. However, the phosgene route has too many obvious drawbacks. With the urgent requirement of environmental protection, synthesis MDI with the non-phosgene route is a front research in the field of green chemistry and chemical engineering. Some key issues of the thermal decomposition of methylene-4,4’-di(methylphenyl-carbamate)(MDC) to synthesize MDI of the non-phosgene route were systematically researched in the dissertation. The achievements and progresses were exhibited as follow: (1) The reaction process and the kinetics of the thermal decomposition of MDC were investigated by the thermal analysis technology. The result showed that the intermediate product methylene-4-(4'-methylphenylcarbamate) phenylisocyanate(MMI) was produced firstly, and then, MDI was manufactured by the thermal decomposition of MMI. The kinetic equation named Valensi equation was determined by the Malek method. The dynamic factors, activation energy(E) and preexponential factor(A), were calculated preliminarily and E was about 249kJ/mol as well as A was about 4.2×1020. (2) It was a difficult problem to quantitatively analyze MMI and MDI. Herein, the purified derivatives with the method of the chromatographic column were analyzed and identified respectively by melting point test, element analysis, 1H nuclear magnetic resonance spectrometry and mass spectrometry. The test results showed that the derivative method with ethanol was credible. And then, an optimal high performance liquid chromatography method named derivative method with ethanol was established. At optimal conditions, the results showed that the correlation coefficient of derivatives of MMI and MDI wasmore than 0.9999 and the relative standard deviation was less than 1.00% respectively in the range of 1～140mg/L. These indicated that the derivative method with ethanol was accurate. (3) The reaction equipments for the thermal decomposition of MDC were researched. Results confirmed that the conversion of MDC was close to 100% and the optimal molar yield of MMI and MDI was 85.0% in the device based on the tubular reactor. When MDC was decomposed in the integrated device of reaction and distillation, the purity of MDI was 79% at the first reaction and distillation. At the second time, the purity of MDI was 92%, as well as the crude yield of MDI was 85%. What’s more, the reaction conditions were milder than the first time. |
| 语种 | 中文 |
| 公开日期 | 2013-09-22 |
| 页码 | 67 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1618]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 姚星星. MDC热分解制备MDI的过程基础研究[D]. 中国科学院研究生院. 2010. |
入库方式： OAI收割
来源：过程工程研究所
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