High-pressure ultraviolet visible near-infrared spectroscopy device for online monitoring of supercritical system

Abstract

The invention relates to a high-pressure ultraviolet visible near-infrared spectroscopy device for online monitoring of a supercritical system. The high-pressure ultraviolet visible near-infrared spectroscopy device comprises a high-pressure reaction kettle, a controller, an ultraviolet visible near-infrared spectrometer or an ultraviolet visible spectrometer and a computer, wherein the ultraviolet visible near-infrared spectrometer or the ultraviolet visible spectrometer is connected with the computer through a conducting wire, the high-pressure reaction kettle is arranged in a sample bin of the ultraviolet visible near-infrared spectrometer or the ultraviolet visible spectrometer, and the high-pressure reaction kettle is connected with the controller through the conducting wire. The high-pressure reaction kettle is communicated with a high-pressure injection pump and a sample introduction metering pump through a feed valve, a sample pipe and a gas-liquid three-way valve, which are mounted on a pipeline, and communicated with a nitrogen bottle and a vacuum pump through an exhaust valve and a gas three-way valve which are mounted on the pipeline. The high-pressure reaction kettle of the high-pressure ultraviolet visible near-infrared spectroscopy device provided by the invention has the advantages of reasonable design, convenience in use, accurate monitoring and the like, and can be used for online monitoring of physical conversion and chemical reaction processes under supercritical conditions.

Description

technical field [0001] The invention belongs to the technical field of high-pressure in-situ ultraviolet-visible-near-infrared spectroscopy monitoring devices, and in particular relates to a high-pressure ultraviolet-visible-near-infrared spectroscopy equipment or device for on-line monitoring of a supercritical system. Background technique [0002] High-pressure in-situ UV-Vis-near-infrared spectroscopy technology can be applied to online monitoring of physical transformation or chemical reaction process in a high-pressure supercritical system under real or near real pressure, temperature and other conditions, to detect the phase behavior of the system and the characteristics of each group. Dynamically monitor the generation of active species and their evolution with pressure, temperature, time, etc., and study the kinetics and mechanism of physical transformation or chemical reaction. This technology plays a unique role in understanding the laws of supercritical systems, o...

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Problems solved by technology

[0003] The literature (The Journal of Supercritical Fluids, 2001, 21, 227-232) reported a high-pressure UV-visible spectroscopy monitoring device. The high-pressure UV-visible sample cell of the device is a single optical path mode, and the high-pressure visible window is made of quartz material, and the maximum volume is less than 2mL , the maximum working pressure does not exceed 20MPa, in addition, the monitoring device cannot achieve stirring during the spectrum test

The existing high-pressure ultraviolet-visible spectroscopy system cannot achieve stirring during the monitoring process, which makes the monitored system substantially different from the real transformation or reaction process, and cannot achieve true in-situ monitoring, resulting in the reliability and reliability of the measurement results. The reliability is low; secondly, the existing high-pressure sample cell is a single optical path mode, which cannot accurately deduct the background or reference absorption during the test process, and cannot meet the needs of online monitoring of some change processes (especially rapid change processes) in the supercritical system ; In addition, the pressure resistance level of the high-pressure sample cell is low, which limits the application of supercritical system ultraviolet-visible spectroscopy technology

Existing high-pressure ultraviolet-visible spectroscopy technology cannot realize direct and effective real-time online monitoring of microscopic dynamic processes under high temperature and high pressure or supercritical systems under real reaction conditions

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