Modular multistage chromatography column as well as sampling method and separating method thereof

Abstract

The invention provides a modular multistage chromatography column as well as a sampling method and a separation method thereof. The modular multistage chromatography column comprises a column top, at least a section of column body and a column bottom which are embedded from top to bottom, a column top sampling hole penetrates through the embedding surface of the column top, an upper sampling hole penetrates through the embedding surface of the upper end of a column body, a lower sampling hole penetrates through the embedding surface of the lower end of the column body, and the lower part of the column body is provided with a sand core, a bottom column sampling hole penetrates through the embedding surface of the column bottom. Compared with the prior art, the modular multistage chromatography column provided by the invention has the following beneficial effects: in the process of separation and purification, the column can be sampled in real time to monitor the separation situation in the column and realize the dynamic monitoring; the number of the column body can be flexibly selected to increase or decrease according to requirements. When the different components are separated in the column body, the column body with different components can be separated, respectively combined with the column top and the column bottom, and assembled into multistage chromatography column for use. The modular multistage chromatography column has the characteristics of high practicability and high flexibility, and wide application ranges.

Description

technical field [0001] The invention relates to a modularized multi-stage chromatographic column and its sampling and separation method, which can be used for real-time sampling and analysis of the liquid in the column and can be separated and combined freely. It is mainly used for separation and purification in chemical experiments, especially in chemical experiments. In organic chemistry experiments, it will be used more widely. Background technique [0002] At present, in the chromatographic columns commonly used in organic chemical synthesis laboratories, the column top, column body and column bottom are integrated and cannot be separated, and the liquid inside the column cannot be sampled and analyzed; the column height is fixed and the specifications are various. During the use of these chromatographic columns, there are many deficiencies. During the separation and purification process, the components in the column cannot be sampled and analyzed, and only the liquid ou...

AI Technical Summary

Problems solved by technology

[0002] At present, in the chromatographic columns commonly used in organic chemical synthesis laboratories, the column top, column body and column bottom are integrated as a whole, which cannot be separated, and the liquid inside the column cannot be sampled and analyzed; the column height is fixed and the specifications are various.

During the use of these chromatographic columns, there are many deficiencies. During the separation and purification process, the components in the column cannot be sampled and analyzed, and only the liquid outlet at the bottom of the column can be used to analyze whether the pure compound is separated. It is full of uncertainties, and there is no way to do anything about the unseparated and pure mixed components. It can only be re-separated and purified, which wastes a lot of resources and labor costs, and greatly affects the efficiency of separation and purification; when separating two compound components with large differences in polarity, When the components with low polarity are separated, the upper undeveloped components cannot be eluted immediately. It is necessary to use a large amount of eluent to make the upper components go through the entire height of the column and separate them from the liquid outlet, which consumes a lot of time. The eluent is not economical and environmentally friendly; when separating compounds with similar polarity, especially isomers, it is difficult to separate, increasing the column height is limited by the height of the chromatographic column, and customizing a higher chromatographic column costs a lot of money Cost, and the utilization rate is not high, and it is also limited by the operating site, so the operation is difficult

The above defects determine that the current chromatography column cannot be economical, environmentally friendly, energy-saving and efficient, and is extremely unsuitable for the current increasingly complex separation system.

[0003] As the requirements for chromatographic separation continue to increase, improvements to chromatographic columns are gradually increasing. For example, in order to flexibly set the height of the chromatographic column and the adsorbent in the separation process, CN201320200721.8 discloses a combined chromatographic column , but it can only be used by freely configuring the number of columns before the separation and purification operation; in order to save the amount of eluent and improve the yield of samples, CN201521102771.8 discloses a combined chromatographic separation column, but it does not solve the problem of How to more effectively determine whether the pure compound is separated in the separation column before the column separation process; in order to achieve column separation and separate elution and separation at the same time, CN201420693338.5 discloses a detachable multi-section chromatography column, but it cannot accurately detect whether the components in the column are separated into different column segments, and it is difficult to overcome the huge vacuum pressure to separate the liquid-filled chromatography column during the separation and purification process, and it is necessary to separate the single column when eluting the products separately The filler in the first-stage column is removed, and the operation steps are increased

Comprehensive analysis, there is no good solution that can detect the separation in the column in time during the separation and purification process of the chromatographic column. According to the detection and analysis results, the column is separated and eluted separately or the number of columns is increased or decreased to continue the purification and separation.

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