固相物质在超临界流体中梯度结晶分离的机理研究

Supercritical fluid crystallization is one of the most interested issue of the application and research field of supercritical fluid these years It has important applied value in the purification, dryness, grain-making, et.al. of non-volatile matters. But it is difficult to purify Solute, especially difficult to the crude biological active components which have close molecular structure and polarity. In our task, we adopted the supercritical fluid extraction and crystalliation technique created by ourselves, make the synchronous purification and separation of crystal ingredients and non-crystal ingredienst in the active components of Chinese traditional medicine become realism, and solved the problem that the crystal ingredients were easy to jam the pipeline in the process of supercritical fluid extraction. This item deal with the Chinese traditional medicines, Ginkgo biloba L. and Andrographis paniculata (Burm.f.), which had remarkable pharmaceutical effect and bright market prospect. By adopting supercritical fluid gradient separation, a new supercritical fluid seperating and purifying technology, extraction and separation of ginkgoliode and andrographolide, the target substances, from other gradients could be realized simultaneously. Moreover, the target substances were displayed on the self-designed crystallization equipment, namely the purity increases gradually from the bottom to the top of the crystallization equipment. If GBE was used as raw material (The percentage of ginkgolides was about 6%), the purity of ginkgolide can reach about 80% after the first supercritical carbon dioxide extraction and crystallization and above 90% the second. The parameters were as follows: temperature, 50-55%; extraction and crystallization pressure: 9-16Mpa; preliminary separation pressure: 5-6Mpa; secondary separation pressure: 3-4Mpa; ratio of height and diameter of the extraction and crystallization container: 6-16; rate of flow: 25L/min. This program investigated the reason, ratio of speed, major influencing factors and degree of supercritical fluid gradient crystallization from many aspects, from which the newly-formed theory of supercritical fluid separation enriches the theoretical basis of this technology. The new technology especially applies to the separation of natural biological activated substance of non-volatile and polar-similar bind. Therefore, it can be widely used to separate and purify the natural substances in the fields such as biology, medicine and pharmaceutics and food. This technology is of the advantages of convenient operation, high speed, low energy-consumation, no pollution and high quality of products, which will contribute to the application of supercritical fluid gradient crystallization and separation in inchistry.

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