对氨基苯基-β-羟乙基砜硫酸酯合成工艺研究  

Study on the Synthesis Process of p-Aminophenyl-β-Hydroxyethyl Sulfone Sulfate

作　　者：蓝晓 LAN Xiao(Guangdong Zhonghe high-tech joint stock company,Maoming,Guangdong 525000)

机构地区：[1]广东众和高新科技股份公司,广东茂名525000

出　　处：《化工生产与技术》2023年第4期15-18,I0003,共5页Chemical Production and Technology

摘　　要：以对硝基氯苯为原料,采用硫醚氧化法制备了对氨基苯基-β-羟乙基砜硫酸酯,讨论了取代还原、缩合、氧化以及酯化反应各阶段反应条件对收率的影响。结果表明,取代还原反应,对硝基氯苯与硫化钠的摩尔比为1∶3、反应时间为7h时为宜;缩合反应,对硝基氯苯与氯乙醇的摩尔比为1∶1.8、溶剂为水时为宜;氧化反应,对氨基苯基-β-羟乙基硫醚与H2O2的摩尔比为1∶2.5、对氨基苯基-β-羟乙基硫与催化剂钨酸钠醚的摩尔比为1∶0.1时为宜;酯化反应,稀释的水量为40mL时为佳(对氨基苯基-β-羟乙基砜硫酸酯的质量为5g)。在此优化条件下制备的对氨基苯基-β-羟乙基砜硫酸酯的质量较好,质量分数、酸值和酯值分别为17.9%、97.76%和97.03%。P-Aminophenyl-β-hydroxyethyl sulfone sulfate was prepared from p-nitrochlorobenzene by thioether oxidation method.The effects of reaction conditions on the yield of substitution reduction,condensation,oxidation and esterification were discussed.The results showed that the molar ratio of p-nitrochlorobenzene to sodium sulfide was 1∶3 and the reaction time was 7 h.In the condensation reaction,the molar ratio of p-nitrochlorobenzene to chloroethanol is 1∶1.8,and the solvent is water.In the oxidation reaction,the molar ratio of p-aminophenyl-β-hydroxyethyl sulfide to H2O2 is 1∶2.5,and the molar ratio of p-aminophenyl-β-hydroxyethyl sulfide to catalyst sodium tungstate ether is 1:0.1.In the esterification reaction,it was better when the diluted water was 40 mL(the mass of p-aminophenyl-β-hydroxyethyl sulfone sulfate was 5 g).The mass fraction,acid value and ester value of p-aminophenyl-β-hydroxyethyl sulfone sulfate prepared under the optimized conditions were 17.9%,97.76%and 97.03%,respectively.

关 键 词：对氨基苯基-β-羟乙基砜硫酸酯 硝基氯苯 取代还原 缩合 氧化 酯化 

分 类 号：TQ247.3[化学工程—有机化工]