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气相SO3磺化法合成染料中间体3-乙氨基-4-甲基苯磺酸
引用本文:张广良,杨效益,郭朝华,沈寒晰.气相SO3磺化法合成染料中间体3-乙氨基-4-甲基苯磺酸[J].印染助剂,2011,28(6).
作者姓名:张广良  杨效益  郭朝华  沈寒晰
作者单位:1. 中国日用化学工业研究院,山西太原,030001
2. 陕西省石油化工研究设计院,陕西西安,710054
摘    要:以N-乙基邻甲苯胺为原料,采用气相SO3磺化法在降膜式磺化反应器中合成染料中间体3-乙氨基-4-甲基苯磺酸,用红外(IR)、电喷雾质谱(ESI-MS)和高效液相色谱(HPLC)对产物进行了表征,结果表明为目标产物.通过滴定法测定磺化产物的中和值,结果表明重复性较好.用中和值计算目标产物质量分数为93.5%,与高效液相色谱分析结果98.2%基本一致,可将中和值作为监测反应进度和产品质量的一个指标.

关 键 词:染料中间体  3-乙氨基-4-甲基苯磺酸  气相SO3磺化法  降膜式磺化反应器  合成

Synthesis of dye intermediate 3-N-ethyl-4-methylbenzenesulfonic acid by gaseous sulfur trioxide sulfonation method
ZHANG Guang-liang,YANG Xiao-yi,GUO Chao-hua,SHEN Han-xi.Synthesis of dye intermediate 3-N-ethyl-4-methylbenzenesulfonic acid by gaseous sulfur trioxide sulfonation method[J].Textile Auxiliaries,2011,28(6).
Authors:ZHANG Guang-liang  YANG Xiao-yi  GUO Chao-hua  SHEN Han-xi
Affiliation:ZHANG Guang-liang1,YANG Xiao-yi1,GUO Chao-hua1,SHEN Han-xi2(1.China Research Institute of Daily Chemical Industry,Taiyuan 030001,China,2.Shanxi Research Design Institute of Petroleum and Chemical Industry,Xi'an 710054,China)
Abstract:Dye intermediate 3-N-ethyl-4-methylbenzenesulfonic acid was synthesized by gaseous sulfur trioxide sulfonation method using N-ethyl-2-methylamiline as raw material in falling film sulfonation reactor.The product was characterized by IR,electro spray ionization-mass spectroscopy(ESI-MS) and high performance liquid dhromatography(HPLC),and the results showed that the product was the target product.The neutralization value of sulfonated products was determined by titration method,and the results indicated good...
Keywords:dye intermediate  3-N-ethyl-4-methylbenzenesulfonic acid  gaseous sulfur trioxide sulfonation method  falling film sulfonation reactor  synthesis  
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