摘要
工业级乙腈通过精制除杂可制备高附加值的高纯乙腈。为开发一种稳定高效的高纯乙腈制备方法,本研究采用氧化、吸附和蒸馏的组合工艺,由工业级乙腈精制得到高纯乙腈,并考察了氧化剂种类及其用量、氧化反应时间、吸附剂种类及其用量、吸附时间、蒸馏出料比(速度比)对产品性能的影响。结果表明,较优的精制工艺条件:氧化剂采用高锰酸钾,用量为原料质量的0.25%,氧化反应时间为2 h;吸附剂采用5A分子筛,其与原料的质量比为1:3,吸附时间为24 h;蒸馏的前馏分、产品和后馏分的出料比控制在1:7:2。在上述条件下,所得高纯乙腈的紫外吸光度和水含量均达到色谱纯(HPLC级)乙腈技术指标和国外市售色谱纯乙腈水平。
High-purity acetonitrile with high added value can be prepared from industrial-grade acetonitrile through impurity removal and purification.To develop a stable and efficient process for the production of high-purity acetonitrile,this study adopted a combined process consisting of oxidation,adsorption,and distillation.Using industrial-grade acetonitrile as the raw material,the effects of oxidant type,dosage,and reaction time;adsorbent type,dosage,and contact time;as well as distillation cut ratios(speed ratio)on product quality were investigated.The results showed that potassium permanganate was the optimal oxidant at a dosage of 0.25%(mass fraction)with a reaction time of 2 h;5A molecular sieves were selected as the adsorbent with a contact time of 24 h and a mass ratio of 1꞉3;the distillation ratio of forecut,product,and tailcut was controlled at 1꞉7꞉2.Under these optimized conditions,the ultraviolet absorbance and water content of the obtained acetonitrile met the technical requirements of Chromatographic purity grade(HPLC-grade)acetonitrile and were comparable to those of commercially available HPLC-grade foreign products.
作者
罗城静彦
裴义霞
LUO Chengjingyan;PEI Yixia(SINOPEC Shanghai Research Institute of Petrochemical Technology Company Limited,Shanghai 201208,China)
出处
《化学反应工程与工艺》
2025年第4期503-509,共7页
Chemical Reaction Engineering and Technology
关键词
色谱纯乙腈
精制
氧化
吸附
蒸馏
chromatographic-grade acetonitrile
refine
oxidation
adsorption
distillation
