基于升华结晶过程的分离精制方法

摘要升华结晶作为一种无溶剂结晶方法,包含了升华和凝华2个过程,即涉及固体-气体-固体的直接相转变过程。其在高纯精品的分离精制、以及物质的新晶型筛选、高质量单晶制备等方面具有极大优势,但因其存在气体的复杂多变性,在理论研究、工业放大和升华设备标准化等方面还存在较大的挑战。针对升华结晶中的升华和凝华2个子过程,对现阶段升华结晶的机理研究进展进行了概括,进一步从晶型、共晶设计、晶体产品分离和纯化等方面总结了升华结晶在分离精制方面的应用,并介绍了几种代表性升华装置。同时,针对现阶段升华结晶的研究态势及所存在的问题,提出了关于深化机理、完善模型的新思路,探讨了升华结晶在高效分离、结晶过程精准控制方面的关键问题和发展方向。

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	苏鑫
	尚泽仁
	余畅游
	高也
	何兵兵
	李康丽
	陈明洋
	龚俊波

关键词：升华结晶凝华机理分离精制升华装置

Abstract： Sublimation crystallization is a solvent-free crystallization method and it involves a composite process of sublimation and desublimation, which means it has a direct phase transition process of solid-gas-solid. It has great advantages in the separation and refinement of high purity products, the screening of new polymorphs and the preparation of high-quality single crystals. However, there are still great challenges in its theoretical research, industrial amplification, and equipment standardization due to the complex variability of gases. This article summarized sublimation crystallization mechanisms and its applications in polymorph control, co-crystal design, separation and purification of crystal product. Several typical sublimation equipment were introduced. Moreover, some new ideas about deepening the mechanism and perfecting the model are proposed, and the key problems and development directions of sublimation crystallization in the application of efficient separation and precise control of crystallization process are discussed.

Keywords： sublimation crystallization desublimation mechanism separation refine sublimation devices

Received 2021-10-16;

Fund:中低品位磷矿及其共伴生资源高效利用国家重点实验室基金(WFKF2018-06);化学和化学工程广东实验室基金(1912014)。

Corresponding Authors: 陈明洋,副研究员,E-mail:chenmingyang@tju.edu.cn;李康丽,博士后,E-mail:kangli_li@163.com。 Email: chenmingyang@tju.edu.cn;kangli_li@163.com

About author: 苏鑫(1997-),女,硕士研究生,现从事工业结晶方面的研究。

引用本文:

苏鑫, 尚泽仁, 余畅游, 高也, 何兵兵, 李康丽, 陈明洋, 龚俊波.基于升华结晶过程的分离精制方法[J]. 化学工业与工程, 2023,40(5): 40-53

SU Xin, SHANG Zeren, YU Changyou, GAO Ye, HE Bingbing, LI Kangli, CHEN Mingyang, GONG Junbo.Separation and refining method based on sublimation crystallization process[J]. Chemcial Industry and Engineering, 2023,40(5): 40-53

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