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A supercritical fluid complexation reaction device with online spectrum monitoring function

A technology of supercritical fluid and complexation reaction, which is applied in measuring devices, color/spectral characteristic measurement, material analysis through optical means, etc. It can solve problems such as uneven heating temperature, affecting spectral monitoring, and high temperature sensitivity. Achieve the effect of precise temperature control, high-quality spectral monitoring data, and easy design structure

Active Publication Date: 2018-04-17
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, the volume of the reactor is small, and it is mainly used to study the spectrum of the complex product, which is difficult to apply to the research on the reaction of constant solid nitrate and complexing agent.
Second, the reactor body is sealed with a flange, which requires a high balance of bolt tightening around the body, so it is inconvenient to open and seal the reactor body, and the sealing reliability is low
Thirdly, electric heating mantle or electric heating belt is mostly used for heating the reactor body, which has the problem of uneven heating temperature, while supercritical CO 2 The system is highly sensitive to temperature, so it is difficult to meet the temperature control requirements
Fourth, the internal structure of the reactor is unreasonable, which is not conducive to the rapid progress of the complexation reaction
Fifth, there is the problem of window material contamination caused by the attachment of solid salt reactants, which affects spectral monitoring; if the problem of window material contamination is alleviated by increasing the distance between the incident window and the exit window, due to the limitation of the spectrometer, only Monitoring of low-concentration reactions, while monitoring of high-concentration reactions is powerless
[0006] Based on the above situation, in order to overcome the shortcomings of the existing supercritical fluid complexation reaction device with online spectrum monitoring function, it is better to meet the requirements of supercritical CO 2 For the application research of extraction and separation of actinides and lanthanides, it is necessary to develop a suitable supercritical fluid complexation reaction device

Method used

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  • A supercritical fluid complexation reaction device with online spectrum monitoring function
  • A supercritical fluid complexation reaction device with online spectrum monitoring function
  • A supercritical fluid complexation reaction device with online spectrum monitoring function

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Adopt the supercritical fluid complexation reaction device of the present invention (the specific structure of the device is as attached Figure 1-2 shown) for supercritical CO 2 The complexation reaction of medium solid neodymium nitrate and tributyl phosphate (TBP) is monitored by online spectrum, and the main monitoring steps are as follows:

[0028] (1) Add solid neodymium nitrate and magnets to the reactor body, tighten the pressure cap of the lid of the kettle, so that the lid of the kettle is sealed with the body of the kettle; connect the rest of the device, and close all valves;

[0029] (2) Open the storage bottle valve, the refrigeration outlet valve, the intake valve, and the discharge valve in sequence, and use CO 2 Exhaust the air inside the reactor and related pipelines;

[0030] (3) Close the storage bottle valve, refrigeration outlet valve, intake valve, and discharge valve, open the thermostat to make the reaction kettle reach the required reaction t...

Embodiment 2

[0040] Adopt the supercritical fluid complexation reaction device of the present invention (the specific structure of the device is as attached Figure 1-2 shown) for supercritical CO 2 The complexation reaction between different solid lanthanide nitrate mixtures and a complexing agent is monitored by online spectroscopy, and the main monitoring steps are as follows:

[0041] (1) Add solid lanthanide nitrate mixture and magnet to the still body of the reactor, tighten the pressure cap of the still cover, so that the still cover is sealed with the still body; connect the rest of the device, and close all valves;

[0042] (2) Open the storage bottle valve, the refrigeration outlet valve, the intake valve, and the discharge valve in sequence, and use CO 2 Exhaust the air inside the reactor and related pipelines;

[0043] (3) Close the storage bottle valve, refrigeration outlet valve, intake valve, and discharge valve, open the thermostat to make the reaction kettle reach the re...

Embodiment 3

[0052] Adopt the supercritical fluid complexation reaction device of the present invention (the specific structure of the device is as attached Figure 1-2 shown) for supercritical CO 2 Online spectroscopic monitoring of the complexation reaction between solid lanthanide and actinide nitrate mixtures and a complexing agent, the main monitoring steps are as follows:

[0053] (1) Add solid lanthanide and actinide nitrate mixture and magnet to the still body of the reactor, tighten the pressure cap of the kettle cover, so that the kettle cover is sealed with the kettle body; connect the rest of the device, and close all valves;

[0054] (2) Open the storage bottle valve, the refrigeration outlet valve, the intake valve, and the discharge valve in sequence, and use CO 2 Exhaust the air inside the reactor and related pipelines;

[0055] (3) Close the storage bottle valve, refrigeration outlet valve, intake valve, and discharge valve, open the thermostat to make the reaction kettl...

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Abstract

The invention belongs to the research field of separation of actinide series elements and lanthanide series elements by a supercritical fluid. In order to overcome the disadvantages of an existing supercritical fluid complex reaction device, the invention provides a supercritical fluid complex reaction device with an online spectrum monitoring function. The device comprises a CO2 storage bottle, a refrigerator, a gas pump, a reaction kettle, a magnetic stirrer, a constant-temperature box, a temperature sensor, a light source, a spectrograph, a data processing system, a reagent bottle, a metering pump and a receiving bottle; and the reaction kettle comprises a kettle body, a kettle cover and a kettle pressing cap. The supercritical fluid complex reaction device provided by the invention has the advantages of rapid supercritical complex reaction speed, capability of rapidly acquiring high-quality spectrum monitoring data, convenience for accurately adding materials and accurately controlling temperatures, high reliability and the like; and application researches of the extraction and separation of the actinide series elements and lanthanide series elements by supercritical CO2.

Description

technical field [0001] The invention belongs to the research field of supercritical fluid extraction and separation of actinides and lanthanides, and in particular relates to a supercritical fluid complexation reaction device with an online spectrum monitoring function. Background technique [0002] Supercritical CO 2 Non-toxic, non-flammable, stable in radiation and chemical properties, it is a green solvent that has attracted much attention and is used to replace organic solvents. Supercritical CO with complexing agent 2 Actinides and lanthanides can be extracted from aqueous solutions, solid substrates, ionic liquids, and solid oxides, and can greatly reduce the volume of radioactive secondary waste liquid. [0003] Research on supercritical CO 2 The separation of actinides and lanthanides, as well as actinides, is of great significance for the popularization and application of this technology. For online monitoring of supercritical CO 2 For the complexation reaction...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/00G01N21/31
CPCB01D11/00G01N21/314
Inventor 朱礼洋王壮飞何辉唐洪彬
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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