摘要
研究了氯化胆碱-尿素低共熔溶剂DES的公斤级放大制备规律。考察了物料配比、反应时间及反应温度对最终产品DES理化性质的影响,分别测定了合成过程中DES折光率、电导率和粘度等性质指标的变化,并通过FT-IR红外光谱分析了DES产品可能的化学结构。实验结果表明,在氯化胆碱与尿素的比例为1∶1时,不能生成DES;氯化胆碱与尿素比例为1∶1.5和1∶2时,均可生成DES;在比例为1∶2的条件下,60℃时不能生成DES,70、80和90℃时均可生成DES,且生成DES的时间随温度的升高而缩短。当DES折光率达到0.6时,其性质趋于稳定,可认为形成了结构稳定的DES。此外还发现,原料和产品中的水含量对DES产品的理化性质有一定程度的影响。本研究澄清了文献报道的DES理化性质存在差异的原因,为工业化放大生产氯化胆碱-尿素DES提供了基础数据。
The deep eutectic solvent(DES) composed of choline chloride and urea was prepared on kilogram level. The molar ratio effect, temperature and reaction time on physi-chemical properties of the DES were investigated, respectively.Refractive index, conductivity, viscosity of samples and products were measured during the reaction process. A possible chemical structure of the DES was analyzed based on FT-IR infrared spectroscopy spectrum. Experimental results show that the deep eutectic solvent can not be formed for the ratio of choline chloride to urea of 1 ∶1 for the ratio of choline chloride to urea of 1∶1.5 and 1∶2, and not formed. In the case of the ration of 1∶2, the deep eutectic solvent can be formed at 70, 80 and 90 ℃, and not at 60 ℃. The required time of the reaction is shortened with the increasing temperature. When refractive index is 1.505, the DES exhibits constant properties, which suggested that a stable chemical structure is formed. In addition, water contents in feedstocks and product affect property of DES in some content. A difference of physichemical properties of DES in literatures was clarified. The study provides valuable data for commercial production of DES.
作者
冯树波
王淑波
候晓夏
张郝朋
翟倩楠
Feng ShuBo;Wang Shubo;Hou Xiaoxia;Zhang Haopeng;Zhai Qiannan(Institute of Petroleum and Chemical Engineering, College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang, 050018, China;Bayin Guoleng Vocational College, Kuerle 841000, China)
出处
《煤炭与化工》
CAS
2019年第9期135-141,共7页
Coal and Chemical Industry
关键词
氯化胆碱
尿素
DES
合成
公斤级放大
choline chloride
urea
DES
synthesis
kilogram scale-up preparation
