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Multistage supercritical fluid rectification separation and continuous flow elution preparation chromatographic separation device

A supercritical fluid, rectification separation technology, applied in distillation separation, solid adsorbent liquid separation, separation methods, etc., can solve the problems of difficult to achieve industrialized continuous production, limited application, affecting separation effect, etc., and achieve easy and intelligent The effect of control, efficient distillation separation, and simple composition of fractions

Active Publication Date: 2019-04-09
厦门昊琦科学仪器有限公司
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  • Abstract
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Problems solved by technology

Supercritical fluid rectification and separation rely solely on temperature gradient adjustment, the adjustable range is limited, and the application is limited; when the temperature of the supercritical fluid rectification tower bottom is too low, it is easy to overflow, and when the tower top temperature is high, it is easy to accumulate material, and the rectification cannot be achieved For large-diameter rectification columns, the external heating of the column forms a temperature gradient from outside to inside, which can easily cause uneven temperature distribution in the same layer in the column and affect the separation effect; for materials with complex compositions, supercritical fluid distillation separation generally cannot achieve To achieve the effect of monomer separation, combined with other chromatographic methods, it is still difficult to achieve the purpose of industrial continuous production

Method used

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  • Multistage supercritical fluid rectification separation and continuous flow elution preparation chromatographic separation device

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Embodiment Construction

[0029] Attached below figure 1 The present invention is further described in detail with specific embodiments.

[0030] The multistage supercritical fluid rectification separation and continuous flow elution preparation chromatographic separation device of the present invention, its separation process comprises the following steps:

[0031] 1. First, make all the fluid transfer pumps, on-off valves, and switching valves in the closed state, and open all the pressure-limiting control valves and back-pressure control valves 21 and 22.

[0032] 2. Turn on the fluid delivery metering pump 61c to pump the supercritical fluid from the inlet of the lower end of the first-stage rectification column 11 into the rectification column, and make it fill the first-stage, second-stage, and third-stage rectification columns, then adjust The back pressure of the back pressure valve 23 is greater than 80MPa.

[0033] 3. Turn on the heater power supply of the first-stage rectification column 1...

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Abstract

A multi-stage supercritical fluid rectification separation and continuous flow elution preparative chromatography separation device consists of a supercritical fluid rectification separation mechanism and a supercritical continuous flow elution preparative chromatography separation mechanism; and supercritical fluid rectification separation mechanism consists of three stages of rectification units and has pressure gradient and temperature gradient. By the device, supercritical fluid rectification can operate and run under the pressure gradient and the temperature gradient simultaneously, the adjusting range of properties such as solubility, permeability and volatility of supercritical fluid is wide, the properties are adjusted accurately, and the rectification separation effect is improved; pressure gradient controlled adjustment is added, and the defects that materials overflow easily when the temperature of the bottom of a supercritical fluid rectification tower is low and the materials are caked easily when the temperature of the top of the tower is high due to pure temperature adjustment can be avoided; and compared with temperature adjustment, pressure adjustment has the characteristics of timely response and zero lagging, and intelligent control is easy to realize.

Description

technical field [0001] The invention relates to a multistage supercritical fluid rectification separation and continuous flow elution preparation chromatographic separation device. Background technique [0002] With the enhancement of people's awareness of environmental protection, green chemistry has become a research hotspot in many scientific and technological fields, and has become the mainstream of new processes, new methods, and new technology development concepts. As a special state of matter above the critical pressure and critical temperature, supercritical fluid has the characteristics of low viscosity of gas, high density of liquid, and a diffusion coefficient between gas and liquid. It has high solubility for substances, Strong permeability, non-toxic, non-flammable, non-chemical corrosive; rich in sources, cheap in price; rapid separation from solute can be realized by changing the phase state only by changing the pressure. It is used in the fields of biomedicin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/14B01D3/34B01D3/42B01D15/40
CPCB01D3/143B01D3/34B01D3/42B01D15/40
Inventor 许建中许晨胡浩
Owner 厦门昊琦科学仪器有限公司
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