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High-pressure in-situ infrared spectroscopy apparatus for monitoring supercritical system on line

An infrared spectrum and infrared spectrometer technology, which is applied in the field of high-pressure in-situ infrared spectrum monitoring devices, can solve the problems of reduced reliability and reliability of measurement results, limited application scope, inability to realize stirring, etc., and achieves improved mass transfer diffusion rate and Test efficiency, overcome the complex structure, and the effect of reasonable design

Inactive Publication Date: 2012-05-02
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this test system (device) are: first, the total reflection crystal at the bottom of the high-pressure infrared sample cell will shift the analysis optical path with the movement of the sample cell. Before the test, the optical path must be calibrated, and the calibration operation is cumbersome
Regardless of the transmission type or the attenuated total reflection type, the existing high-pressure in-situ infrared spectroscopy system cannot achieve stirring during the monitoring process, which makes the monitored system substantially different from the real transformation or reaction process, making the measurement results reliable and reliable. Reduced reliability
In addition, the low pressure level of the in-situ infrared sample cell limits the application range of high-pressure / supercritical system in-situ infrared spectroscopy

Method used

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  • High-pressure in-situ infrared spectroscopy apparatus for monitoring supercritical system on line
  • High-pressure in-situ infrared spectroscopy apparatus for monitoring supercritical system on line
  • High-pressure in-situ infrared spectroscopy apparatus for monitoring supercritical system on line

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Effect test

Embodiment 1

[0021] exist figure 1 Among them, the high-pressure in-situ infrared spectroscopy device for on-line monitoring of supercritical systems in this embodiment consists of a high-pressure injection pump 1, a metering pump 2, a gas-liquid three-way valve 3, a nitrogen cylinder 4, a nitrogen three-way valve 5, a vacuum pump 6, and a pressure sensor 7. Injection valve 8, exhaust valve 9, infrared sensor 10, optical fiber 11, reflection chamber 12, computer 13, infrared spectrometer 14, high pressure reactor 15, temperature measuring thermocouple 16, heater 17, electromagnetic stirrer 18 , temperature control thermocouple 19, controller 20, sealing pressure cap 21, sealing ferrule 22, and sealing joint 23 are connected to form.

[0022]An electromagnetic stirrer 18 is installed under the lower surface of the high-pressure reactor 15, and the electromagnetic stirrer 18 is connected to the governor 20-1 on the controller 20 through a wire, and the governor 20-1 controls the operating st...

Embodiment 2

[0027] The attenuation total reflection prism 10-2 of the infrared sensor 10 of the present embodiment is a single crystal silicon crystal attenuation total reflection prism, the front end part of the optical fiber 11 penetrates into the inner cavity of the sensor housing 10-1, and the end of the optical fiber 11 is bonded to the The upper end face of the attenuated total reflection prism 10-2. The shape of the present embodiment attenuating total reflection prism 10-2 is a conical prism at the top, and the bottom is a triangular prism whose side is connected with the bottom surface of the conical truncated body. The angle α between the other two side attenuated total reflection detection planes R1 and attenuated total reflection detection plane R2 is 90°. The other components and the connection relationship of the components are the same as in Embodiment 1. The performance parameters of the high-pressure in-situ infrared spectroscopy device for on-line monitoring of the supe...

Embodiment 3

[0029] The attenuation total reflection prism 10-2 of the infrared sensor 10 of the present embodiment is a single crystal silicon crystal attenuation total reflection prism, the front end part of the optical fiber 11 penetrates into the inner cavity of the sensor housing 10-1, and the end of the optical fiber 11 is bonded to the The upper end face of the attenuated total reflection prism 10-2. The shape of the attenuating total reflection prism 10-2 of the present embodiment is a frustum of a cone, and the bottom is a triangular prism whose side is connected with the bottom of the frustum of a cone. The angle α between the other two side attenuated total reflection detection planes R1 and attenuated total reflection detection plane R2 is 90°. The other components and the connection relationship of the components are the same as in Embodiment 1. The performance parameters of the high-pressure in-situ infrared spectroscopy device for on-line monitoring of the supercritical sys...

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Abstract

A high-pressure in-situ infrared spectroscopy apparatus for monitoring a supercritical system on line comprises a high-pressure reaction kettle, a controller, an infrared spectrometer and a computer, a sample intake valve and a three-way gas-liquid valve of the high-pressure reaction kettle communicate with a high-pressure injection pump, the high-pressure reaction kettle communicates with a metering pump through the sample intake valve and the three-way gas-liquid valve, communicates with a nitrogen cylinder and a vacuum pump through an exhaust valve and a three-way nitrogen valve and communicates with a pressure sensor through a pipeline, a temperature-measuring thermocouple which is connected with the temperature indicator of the controller through a wire is arranged on the high-pressure reaction kettle, a heater and a temperature-controlling thermocouple which are connected with the temperature controller of the controller through wires are arranged on the high-pressure reaction kettle, the pressure sensor is connected with the pressure indicator of the controller through a wire, and the infrared spectrometer is connected with the computer through a wire. The high-pressure in-situ infrared spectroscopy apparatus also comprises an electromagnetic agitator, an emission bin and an optical fiber, the electromagnetic agitator is arranged under the high-pressure reaction kettle and connected with the speed regulator of the controller, the emission bin is arranged on the infrared spectrometer, and the optical fiber is connected with the emission bin and an infrared sensor inserted into the high-pressure reaction kettle.

Description

technical field [0001] The invention belongs to the technical field of high-pressure in-situ infrared spectroscopy monitoring devices, and in particular relates to a high-pressure in-situ infrared spectroscopy equipment or device for on-line monitoring of a supercritical system. Background technique [0002] High-pressure in-situ 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 and temperature conditions, and to detect the phase behavior of the system and the relationship between components. 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. It plays a unique role in understanding the laws of supercritical systems, optimizing process parameters, regulating process results, and promot...

Claims

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Application Information

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IPC IPC(8): G01N21/35G01N21/01
Inventor 刘昭铁陈建刚刘璇刘忠文
Owner SHAANXI NORMAL UNIV
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