制氨系统尿素质量分数测定方法改进
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摘要
针对锅炉烟气脱硝系统还原剂氨的制备过程中尿素原料的质量分数测试,在GB/T2441.1—2008蒸馏后滴定法测定尿素总氮质量分数的基础上,结合尿素溶液测定方法,形成改进化学法。实验采集电厂某脱硝系统还原剂制备装置的尿素原料为实验样品,采用改进化学法获得的尿素质量分数为99.56%,与蒸馏后滴定法的结果相符;改进化学法获得的尿素质量分数与结合样品中缩二脲和亚甲基二脲质量分数反推出?、?、?值的标准计算法结果一致。结果表明,改进化学法准确可靠,可快速获得不同批次尿素质量分数,为现场工作提供数据依据。
This paper focuses on detecting the mass fraction of urea during the preparation of ammonia, the reducing agent of flue gas denitration system in boilers. On the basis of post-distillation titration method in GB/T2441.1—2008 for determining the total nitrogen content of urea, and combining with the approach of urea solution test method, an improved chemical method was proposed to detect the urea content. Moreover, this method was applied to measure the mass fraction of the urea collected from ammonia preparation device of a power plant, and the value was 99.56%, which is consistent with that by the distillation titration method. Besides,this result also agrees with that obtained by the standard method(Back deriving the ?, ? and ? values by using mass fraction of biuret and methylene diurea in the sample). The improved chemical detection method is accurate,reliable and can obtain the mass fraction of urea from different batches rapidly, which can provides data basis for field work.
This paper focuses on detecting the mass fraction of urea during the preparation of ammonia, the reducing agent of flue gas denitration system in boilers. On the basis of post-distillation titration method in GB/T2441.1—2008 for determining the total nitrogen content of urea, and combining with the approach of urea solution test method, an improved chemical method was proposed to detect the urea content. Moreover, this method was applied to measure the mass fraction of the urea collected from ammonia preparation device of a power plant, and the value was 99.56%, which is consistent with that by the distillation titration method. Besides,this result also agrees with that obtained by the standard method(Back deriving the ?, ? and ? values by using mass fraction of biuret and methylene diurea in the sample). The improved chemical detection method is accurate,reliable and can obtain the mass fraction of urea from different batches rapidly, which can provides data basis for field work.
引文
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[2]RAHIMPUR M R.A non-ideal rate-based model for industrial urea themal hydrolyser[J].Chemical Engineering and Processing,2004,43(10):1299-1307.
[3]KOEBEL M,ELSENER M,KLEEMANN M.Urea-SCR:apromising technique to reduce NOx emissions from automotive diesel engines[J].Catalysis Today,2000,59(3/4):335-345.
[4]姚宣,沈滨,郑鹏.烟气脱硝用尿素水解装置性能分析[J].中国电机工程学报,2013,33(14):38-43.YAO Xuan,SHEN Bin,ZHENG Peng.Characteristics of urea hydrolysis equipment for flue gas denitration[J].Proceedings of the CSEE,2013,33(14):38-43.)
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[12]DENTE M,ROVAGLIO M,BOZZANO G,et al.Gas-liquid reactor in the synthesis of urea[J].Chemical Engineering Science,1992,47(9):2475-2480.
[13]RAHIMPOUR M R.A non-ideal rate-based model for industrial urea thermal hydrolyser[J].Chemical Engineering and Processing:Process Intensification,2004,43(10):1299-1307.
[14]魏顺安,杨楠,付雪梅,等.尿素溶液分离体系的汽液平衡[J].化学工程,2011,39(11):83-87.WEI Shun’an,YANG Nan,FU Xuemei,et al.Vapor-liquid equilibrium of urea solution separation system[J].Chemical Engineering,2011,39(11):83-87.
[15]WEI S A,ZHANG H J.Calculation of H2O-NH3-CO2vapor liquid equilibria at high concentration conditions[J].Chinese Journal of Chemical Engineering,2004,12(1):134-136.
[16]MAHALIK K,SAHU J,PATWARDHAN A V,et al.Kinetic studies on hydrolysis of urea in a semi-batch reactor at atmospheric pressure for safe use of ammonia in a power plant for flue gas conditioning[J].Journal of Hazardous Materials,2010,175(1):629-637.
[17]张向宇,高宁,张波,等.高浓度尿素水解制氨试验研究[J].热力发电,2016,45(6):57-62.ZHANG Xiangyu,GAO Ning,ZHANG Bo,et al.Experimental study on ammonia preparation by high concentration urea hydrolysis[J].Thermal Power Generation,2016,45(6):57-62.
[18]杨伟群.酸碱滴定终点误差分析[J].化学与粘合,2007(1):68-71.YANG Weiqun.Analysis of the endpoint error in acidbase titration[J].Chemistry and Adhesion,2007(1):68-71.
[19]林树昌.定量分析化学[M].北京:北京师范大学出版社,1991:45.LIN Shuchang.Analysis of the endpoint error in acid-base titration[M].Beijing:Beijing Normal University Press,1991:45.
[20]中国寰球化学工程公司.氮肥工艺设计手册.尿素[M].北京:化学工业出版社,1993:48.China Global Chemical Engineering Co.,Ltd.Manual for design of nitrogen fertilizer process[M].Beijing:Chemical Technology Press,1993:48.
[21]中华人民共和国国家质量监督检验检疫总局.尿素:GB 2440-2001[S].北京:中国标准出版社,2001.General Administration of Quality Supervision,Inspection and Quarantine of the people’s Republic of China.Urea:GB 2440-2001[S].Beijing:Standards Press of China,2001.
[22]中华人民共和国国家质量监督检验检疫总局.尿素的测定方法第2部分:缩二脲含量分光光度法GB/T2441.2-2010[S].北京:中国标准出版社,2010.General Administration of Quality Supervision,Inspection and Quarantine of the people’s Republic of China.Determination of urea:part 2:biuret content:spectrophotometric method[S].Beijing:Standards Press of China,2010.
[23]中华人民共和国国家质量监督检验检疫总局.尿素的测定方法第3部分:水分卡尔·费休法:GB/T2441.3-2010[S].北京:中国标准出版社,2010.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China.Determination of urea:part 3:water content:Karl Fischer method:GB/T 2441.3-2010[S].Beijing:Standards Press of China,2010.
[2]RAHIMPUR M R.A non-ideal rate-based model for industrial urea themal hydrolyser[J].Chemical Engineering and Processing,2004,43(10):1299-1307.
[3]KOEBEL M,ELSENER M,KLEEMANN M.Urea-SCR:apromising technique to reduce NOx emissions from automotive diesel engines[J].Catalysis Today,2000,59(3/4):335-345.
[4]姚宣,沈滨,郑鹏.烟气脱硝用尿素水解装置性能分析[J].中国电机工程学报,2013,33(14):38-43.YAO Xuan,SHEN Bin,ZHENG Peng.Characteristics of urea hydrolysis equipment for flue gas denitration[J].Proceedings of the CSEE,2013,33(14):38-43.)
[5]YIM S D,KIM S J,BAIK J H,et al.Decomposition of urea into NH3 for SCR process[J].Industrial and Engineering Chemistry Research,2004,43(16):4855-4863.
[6]PARK Y H.An investigation of urea decomposition and selective non-catalytic removal of nitric oxide with urea[D].Texas A&M University,2003:33.
[7]刘志刚,赵庆良,孙丽欣,等.PDAB比色法直接测定液相中的常量尿素[J].哈尔滨工业大学学报,2008,40(8):1214-1217.LIU Zhigang,ZHAO Qingliang,SUN Lixin,et al.Determination of medium concentration urea in solution by p-dimethylam inobenzaldehyde colorimetry[J].Journal of Harbin Institute of Technology,2008,40(8):1214-1217.
[8]郑丽行,樊小林,刘刚,等.折光率测定尿素含量的方法研究[J].西北农林科技大学学报(自然科学版),2010,38(12):93-98.ZHENG Lixing,FAN Xiaolin,LIU Gang,et al.Study on refractive index method for determination of urea concentration[J].Journal of Northwest A&F University,2010,38(12):93-98.
[9]施伟红.改良二乙酰一肟-安替比林法测定游泳水中尿素[J].中国卫生检验杂志,2008,18(7):1319-1320.SHI Weihong.Simulaneous determination of urea in swimming water by diacetylmonoxime antipyrine[J].Chinese Journal of Health Laboratory Technology,2008,18(7):1319-1320.
[10]王美兰,贺萍,许卉,等.甲醛法测定尿素总氮含量的若干问题[J].大学化学,2002,17(6):35-37.WANG Meilan,HE Ping,XU Hui,et al.Determination of total nitrogen in urea by formaldehyde method[J].University Chemistry,2002,17(6):35-37.
[11]中华人民共和国国家质量监督检验检疫总局.尿素的测定方法第1部分:总氮含量:GB/T 2441.1-2008[S].北京:中国标准出版社,2008.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China.Determination of urea:part 1:total nitrogen content:GB/T 2441.1-2008[S].Beijing:Standards Press of China,2008.
[12]DENTE M,ROVAGLIO M,BOZZANO G,et al.Gas-liquid reactor in the synthesis of urea[J].Chemical Engineering Science,1992,47(9):2475-2480.
[13]RAHIMPOUR M R.A non-ideal rate-based model for industrial urea thermal hydrolyser[J].Chemical Engineering and Processing:Process Intensification,2004,43(10):1299-1307.
[14]魏顺安,杨楠,付雪梅,等.尿素溶液分离体系的汽液平衡[J].化学工程,2011,39(11):83-87.WEI Shun’an,YANG Nan,FU Xuemei,et al.Vapor-liquid equilibrium of urea solution separation system[J].Chemical Engineering,2011,39(11):83-87.
[15]WEI S A,ZHANG H J.Calculation of H2O-NH3-CO2vapor liquid equilibria at high concentration conditions[J].Chinese Journal of Chemical Engineering,2004,12(1):134-136.
[16]MAHALIK K,SAHU J,PATWARDHAN A V,et al.Kinetic studies on hydrolysis of urea in a semi-batch reactor at atmospheric pressure for safe use of ammonia in a power plant for flue gas conditioning[J].Journal of Hazardous Materials,2010,175(1):629-637.
[17]张向宇,高宁,张波,等.高浓度尿素水解制氨试验研究[J].热力发电,2016,45(6):57-62.ZHANG Xiangyu,GAO Ning,ZHANG Bo,et al.Experimental study on ammonia preparation by high concentration urea hydrolysis[J].Thermal Power Generation,2016,45(6):57-62.
[18]杨伟群.酸碱滴定终点误差分析[J].化学与粘合,2007(1):68-71.YANG Weiqun.Analysis of the endpoint error in acidbase titration[J].Chemistry and Adhesion,2007(1):68-71.
[19]林树昌.定量分析化学[M].北京:北京师范大学出版社,1991:45.LIN Shuchang.Analysis of the endpoint error in acid-base titration[M].Beijing:Beijing Normal University Press,1991:45.
[20]中国寰球化学工程公司.氮肥工艺设计手册.尿素[M].北京:化学工业出版社,1993:48.China Global Chemical Engineering Co.,Ltd.Manual for design of nitrogen fertilizer process[M].Beijing:Chemical Technology Press,1993:48.
[21]中华人民共和国国家质量监督检验检疫总局.尿素:GB 2440-2001[S].北京:中国标准出版社,2001.General Administration of Quality Supervision,Inspection and Quarantine of the people’s Republic of China.Urea:GB 2440-2001[S].Beijing:Standards Press of China,2001.
[22]中华人民共和国国家质量监督检验检疫总局.尿素的测定方法第2部分:缩二脲含量分光光度法GB/T2441.2-2010[S].北京:中国标准出版社,2010.General Administration of Quality Supervision,Inspection and Quarantine of the people’s Republic of China.Determination of urea:part 2:biuret content:spectrophotometric method[S].Beijing:Standards Press of China,2010.
[23]中华人民共和国国家质量监督检验检疫总局.尿素的测定方法第3部分:水分卡尔·费休法:GB/T2441.3-2010[S].北京:中国标准出版社,2010.General Administration of Quality Supervision,Inspection and Quarantine of the People’s Republic of China.Determination of urea:part 3:water content:Karl Fischer method:GB/T 2441.3-2010[S].Beijing:Standards Press of China,2010.
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