摘要
以质量分数30%的过氧化氢溶液为氧化剂、甲酸为催化剂,结合蒸馏工艺脱除α-甲基萘中的甲基苯并噻吩,考察了甲酸和过氧化氢用量、反应温度、反应时间、原料中氮化物等因素对脱硫率的影响。实验结果表明,在反应温度为40~80℃时,升高反应温度有利于提高脱硫率;最佳反应条件为:温度70℃、n(HCOOH):n(S)=5.8、n(H2O2):n(S)=8.6、反应时间60min,此时脱硫率可达100.00%;原料中的氮化物会与甲酸形成络合物,降低脱硫率;利用α-甲基萘与反应产物之间较大的沸点差异,经过简单蒸馏,即可彻底去除反应中生成的噻吩砜或亚砜,精制后的α-甲基萘纯度提高了2%~3%,总收率大于95%,并由原来的淡黄色变为无色透明。
Oxidative desulphurization of 1 -methylnaphthalene with mass fraction 30% hydrogen peroxide solution as oxidant and formic acid as catalyst was investigated. Methyl -benzothiophene in 1 -methylnaphthalene was removed by successive distillation. Effects of hydrogen peroxide dosage, formic acid dosage, reaction temperature, reaction time and existence of nitrides in raw material on desulphurization rate were studied. In temperature range of 40 - 80 ℃, the desulphurization rate increases with rising of reaction temperature. Under optimal conditions: n (HCOOH) : n ( S ) 5.8, n (H2O2) : n(S) 8.6,70 ℃ and 60 min,desulphurization rate mounts to 100.00%. Nitrides in the raw material combine with formic acid to form complex, which causes the decline of desulphurization rate. After oxidation, the resulted sulfone or sulfoxide can be easily removed from 1 - methylnaphthalene by simple distillation. Purity of 1 -methylnaphthalene can increased by 2% -3% and total yield exceed 95 %. The product becomes colorless and transparent.
出处
《石油化工》
EI
CAS
CSCD
北大核心
2007年第6期614-617,共4页
Petrochemical Technology
基金
北京市属市管高校人才强教计划资助项目(BJJWR20051102)
关键词
Α-甲基萘
氧化脱硫
过氧化氢
甲酸
甲基苯并噻吩
1 - methylnaphthalene
oxidative desulphurization
hydrogen peroxide
formic acid
methyl - benzothiophene