胺光气化法副产焦油中甲苯二胺分离回收及其鉴别
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摘要
研究了胺光气化法副产焦油的分离工艺及邻、间位甲苯二胺(TDA)组成,采用降膜蒸发技术考察了压力、温度、转速、滴速对焦油中邻、间位甲苯二胺含量的影响,通过正交实验优化工艺条件,对焦油轻重组分中的TDA进行鉴别,优化分析条件.结果表明,优化的分离条件为温度200℃、压力15 k Pa、转速参数30 r/min、进料速率1.5m L/min,该条件下甲苯二胺分离效果最佳,相对标准偏差为1.1%～1.5%.
This work investigated the separation process and contents of ortho toluene diamine(O-TDA), metra toluene diamine(B-TDA) of by-product tar of amine light gasification. We discussed the effect of the pressure, temperature, speed, dripping speed on O-TDA, B-TDA contents in tar coupling with the falling film evaporation technology. The contents of TDA in the tar were quantitative identified by orthogonal experiment optimization. The results show that the optimal separation conditions are at temperature of 200 ℃, 15 k Pa pressure, rotating speed of 30 r/min, and the feed rate of 1.5 r/min, then the separating efficiency is best with a relative standard deviation of 1.1%～1.5%.
This work investigated the separation process and contents of ortho toluene diamine(O-TDA), metra toluene diamine(B-TDA) of by-product tar of amine light gasification. We discussed the effect of the pressure, temperature, speed, dripping speed on O-TDA, B-TDA contents in tar coupling with the falling film evaporation technology. The contents of TDA in the tar were quantitative identified by orthogonal experiment optimization. The results show that the optimal separation conditions are at temperature of 200 ℃, 15 k Pa pressure, rotating speed of 30 r/min, and the feed rate of 1.5 r/min, then the separating efficiency is best with a relative standard deviation of 1.1%～1.5%.
引文
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[2]Bokhari J,Muhammad K R.Evaluation of Anti-asthmatic and Antioxidant Potential of Boerhavia Procumbens in Toluene Diisocyanate(TDI)Treated Rats[J].J.Ethnopharmacol.,2015,172:377-385.
[3]De Lorenzi E,Massolini G,Macchia M,et al.HPLC Determination of Urinary 2,4-and 2,6-Toluene Diamines as Potential Degradation Products of Polyurethane Breast Implants[J].Chromatographia,1995,41(5/6):661-664.
[4]李玉刚,李晓明,强光明,等.甲苯二胺精制过程节能改造的有效能分析[J].过程工程学报,2004,4(5):406-409.
[5]于正一,李大鹏,贾培世,等.从焦油中回收甲苯二胺的方法[P].中国专利:103896780B,2015-08-19.
[6]De Lorenzi E,Massolini G,Gangini C,et al.Development of an Ion-pair HPLC Method for the Determination of 2,4-and2,6-Toluene Diamine in Human Plasma[J].Chromatographia,1998,47(2):84-88.
[7]Schettgen T,Heinrich K,Kraus T.Determination of2,5-Toluylenediamine(2,5-TDA)and Aromatica Mines Inurine after Personal Application of Hairdues:Kineticandose[J].Tananla,2011,5(2):127-133.
[8]Yeh H J,Lin W C,Sheu S C,et al.Microwave-assisted Acid Hydrolysis of Toluene Diamine Conjugates in Urine Samples for Biomarkers in Toluene Diisocyanate Analysis[J].Talanta,2007,72(4):1527-1532.
[9]Fu Y,Mo H Y,Gao W,et al.Affinity Selection-based Two-dimensional Chromatography Coupled with High-performance Liquid Chromatography-mass Spectrometry for Discovering Xanthine Oxidase Inhibitors from Radix Salviae Miltiorrhizae[J].Anal.Bioanal.Chem.,2014,406(4):4987-4995.
[10]John J,Frederick G,Peter S,et al.Efficacy and Safety of the Oraneuraminidase Inhibitor Osetamivir in Treating Acute Influenza[J].Japan Automobile Manufacturers Association,2002,283(8):1016-1019.
[11]John C R,Kenneth M K,Michael J P,et al.Practical Total Synthesisof the Anti-influenza Drug GS-4104[J].J.Org.Chem.,1998,63(2):4545-4550.
[12]Federspiel M,Fischer R,Hennig M,et al.Industrial Synthesis of the Key Precursor in the Synthesis of the Anti-influenza Drug Oseltamivir Phosphate Ro 64-0796/002[J].Org.Process Res.Dev.,1999,3(1):266-270.
[13]Becker M W,Chapman H H,Kelly D E,et al.Manufacture of Cyclohexenecarboxylate Esters and Intermediates[P].WO Pat.:995566,1999-11-14.
[14]Zhu B,Morioka M,Nakamura H,et al.A New Antitumor Antibiotic Dioxolamycin[J].J.Antibiotechnol.,1984,37(6):673-674.
[15]Klaus M H.The Shikimate Pathway Early Steps in the Biosynthesis of Aromatic Compounds[J].Plant Cell,1995,7(7):907-919.
[16]Bharathi A,Wang Y H,Troy J,et al.Determination of Shikimic Acidin Fruits of Illicium Species and Various Other Plant Samples by LC-UV and LC-ESI-MS[J].Chromatographia,2009,69(3):307-314.
[17]Liu H C,Li Q W,Zhang Y,et al.Analysis of Shikimic Acid in Chinese Star Anise by GC-MS with Selected Ion Monitoring[J].Chromatographia,2009,69(3):339-345.
[18]Shen Z,Sun Z,Wu L,et al.Rapid Method for the Determination of Amino Acids in Serum by Capillary Electrophoresis[J].J.Chromatogr.A,2002,979(3):227-232.
[19]王鹏,孙杨,刘哲益,等.薄层色谱-热辅助水解甲基化-气相色谱法测定生化柴油中的甘油酯[J].分析化学,2011,39(9):1427-1431.
[20]陈晓婷,张庆合,李秀琴,等.热重-气相色谱/质谱联用方法鉴别回收油[J].分析化学,2015,43(6):843-848.