湿法脱硫中多硫离子分离方法的建立
Establishment of separation method for polysulfide ions in wet desulfurization
高康 1张弦 1陈帅军 2武喜明 2申峻 1王玉高 1牛艳霞1
作者信息
- 1. 太原理工大学化学工程与技术学院,山西太原 030024
- 2. 山西安弘检测技术有限公司,山西太原 030008
- 折叠
摘要
多硫离子S2是湿式催化氧化脱硫技术中H2S向单质硫转化的中间产物,在脱硫环境中,析硫反应和副盐反应存在平行竞争关系,Sx2-的存在形态及浓度是评价两个竞争反应程度的前提条件.本文通过紫外-可见分光光度法(UV-vis)、液相色谱-质谱仪(LC-MS)和高效液相色谱(HPLC)方法可实现对Sx2-的存在形态及各形态浓度定量测定的目标.结果表明:UV-vis法可测定出Sx2-的总浓度;甲基化法可将Sx2-的各个形态进行捕捉,LC-MS和HPLC法可将各形态的甲基化多硫化物分离,且S2-的硫原子数(2-10)越大保留时间越长;结合UV-vis建立的标准曲线和HPLC上各个形态Sx2-出峰的相对强度,推算出溶液中各形态Sx2-的绝对浓度;多硫化钠溶液主要以S42-、S52-、S62-、S102-为主,其中浓度和pH对Sx2-的影响较小,而温度过高不利于Sx2-的生成,从而不利于单质硫的生成.这一项工作为进一步从源头上研究副盐成因及加快析硫反应的研究奠定了基础.
Abstract
Polysulfide ion Sx2- is an intermediate product of the conversion of H2S to elemental sulfur in wet catalytic oxidation desulfurization technology.In the desulfurization environment,there is a parallel competition between the sulfur evolution reaction and parasite reaction,and the existing form and concentration of Sx2- are the prerequisite for evaluating the degree of the two competitive reactions.In this paper,UV-vis,LC-MS,and HPLC methods were used to determine the existence and concentration of Sx2-.The results showed that the total concentration of Sx2- could be determined by the UV-vis method.The methylation method could capture each form of Sx2-,LC-MS and HPLC methods could separate each form of methylated polysulfide,and the larger the number of sulfur atoms(2-10)of Sx2-,the longer the retention time.Combined with the standard curve established by UV-vis and the relative intensity of each form of Sx2- on HPLC,the absolute concentration of each form of S2-in solution was calculated.S42-,S52-,S62- and S102- were the main types of sodium polysulfide solution,in which the concentration and pH had little effect on Sx2-,and the high temperature was not conducive to the formation of Sx2-,thus not conducive to the formation of elemental sulfur.This work laid a foundation for further research on the origin of parasites and the acceleration of sulfur evolution.
关键词
多硫离子/湿法脱硫/硫化钠Key words
polysulfide ions/wet desulfurization/sodium sulfide引用本文复制引用
出版年
2024