CN112730238A - Supercritical in-situ spectral reaction device - Google Patents
Supercritical in-situ spectral reaction device Download PDFInfo
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- CN112730238A CN112730238A CN202011373575.XA CN202011373575A CN112730238A CN 112730238 A CN112730238 A CN 112730238A CN 202011373575 A CN202011373575 A CN 202011373575A CN 112730238 A CN112730238 A CN 112730238A
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Abstract
The invention discloses a supercritical in-situ spectral reaction device, which comprises a gas path system, a heating system, a water cooling system, a sample cover and a light supply device, wherein the gas path system is connected with the heating system; the outside of the heating system is wrapped with a water cooling system for cooling the heating system; the interior of the heating system is communicated with the gas output end of the gas path system, and the gas path system provides required test pressure for the heating system through gas pressure; the light supply device penetrates through a heating area of the heating system; the sample cover is fixed at the front end of the light supply device for providing light sources with different spectrums; a sample cavity for placing a sample is formed in the center of the sample cover; according to the invention, the light is controlled by the light supply device, so that the influence of an external light source on the test is reduced, and the test accuracy is improved.
Description
Technical Field
The invention relates to the technical field of material structure-mechanism in-situ characterization, in particular to a supercritical in-situ spectral reaction device.
Background
The structural study of the disordered state of a substance under extreme pressure and temperature conditions is an attractive scientific field. The reason is to characterize the importance of temperature and pressure dependence of the material structure to gain insight into the key bonding interactions. Most typical of these is the study of the solubility of metal ions in solution. Such as the reported deep analysis of the solubility and morphology of Cu ions in aqueous fluids at different PH ranges, different temperature and pressure conditions ranges. Hemley et al measured the solubility of Cu in a 1 molar chloride solution at temperatures ranging from 300 to 500 ℃ and pressures of 50, 100 and 200MPa, and found that it decreased slightly with increasing temperature and pressure. A sample of an aqueous solution of metallic copper + heated to 325-600 ℃ at 30MPa was analyzed by Louvel et al using the same technique and reported that the addition of sulfur to 0.15mol HCl resulted in a Cu solubility decrease from 4254 + -70 ppm to 670ppm at 325 ℃. Similar studies are also numerous, and the most important concern is the structural changes of substances under different supercritical reaction conditions. However, the research on the structural change needs to provide an environment of ultra-high pressure and ultra-high temperature, and generally needs a set of matched physical characterization means to realize the structural research. With the advent of synchrotron sources that can provide very bright and well focused beams, the compatibility of supercritical equipment with ultra-high temperature and ultra-high pressure conditions with X-ray spectroscopy techniques, such as X-ray diffraction, small angle scattering, X-ray absorption spectroscopy, etc., has also gradually become well established. For example, researchers at the university of cantonese, guangdao, in rural area have developed an autoclave device with high temperature and high pressure, which can realize the research of several X-ray absorption spectra sXAS and small-angle X-ray scattering sxss under high temperature and high pressure in a certain sense, and once they have used the autoclave device to intensively research the structural change relationship between the liquid and metal ions in the aqueous solution under the supercritical condition. In this experiment, researchers have also elaborated how difficult the supercritical reaction conditions can be combined with the experimental difficulties of X-ray techniques (especially using X-ray absorption spectroscopy with high temperature/high pressure sample environments). In addition to the drawbacks of the technique itself, researchers in our country are also subject to the blockade of foreign technologies, and even under similar experimental conditions, the researchers in our country cannot achieve the blockade, so that it is necessary and meaningful for the researchers to develop a supercritical reaction device suitable for synchrotron radiation light sources, even common laboratory light sources.
Aiming at supercritical reaction, two important indexes needed are ultrahigh temperature and ultrahigh pressure, and at present, a plurality of devices can meet the supercritical reaction conditions, including domestic and foreign devices, and can meet various requirements of researchers. However, the biggest problem of the existing equipment and device is that no spectroscopic characterization means can be provided, which brings a certain confusion to researchers in studying the structural state of the substance under the supercritical reaction condition: researchers cannot study the structure of a substance under real and effective high-temperature and high-pressure conditions, and can only estimate a structural change characteristic of the substance by the substance study after unloading the temperature or the pressure, but the structure study under the conditions is obviously distorted and is inaccurate.
For example, in a comparison document CN209537398U, an evaluation system for supercritical depolymerization of residual oil is disclosed, in which a heating device and a pressure device are provided, but the influence of light is not taken into consideration, and inaccurate test results are easily generated.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to build a set of supercritical in-situ spectrum reaction device capable of realizing in-situ spectrum characterization test under the condition of high temperature and high pressure.
In order to solve the technical problems, the invention provides the following technical scheme: the supercritical in-situ spectral reaction device comprises a gas path system, a heating system, a water cooling system, a sample cover and a light supply device; the outside of the heating system is wrapped with a water cooling system for cooling the heating system; the interior of the heating system is communicated with the gas output end of the gas path system, and the gas path system provides required test pressure for the heating system through gas pressure; the light supply device penetrates through a heating area of the heating system; the sample cover is fixed at the front end of the light supply device for providing light sources with different spectrums; the center of the sample cover is provided with a sample cavity for placing a sample.
Preferably, the gas path system comprises an unloading valve, a first ball valve, a tee joint, a pressure gauge, a clamping sleeve and a second ball valve; the unloading valve, the pressure gauge and the second ball valve are sequentially connected to the gas through pipe; the tee joint is communicated with a branch pipe through a sleeve; the branch pipe is provided with a first ball valve; the pressure gauge is connected to the gas through pipe through a four-way joint; the other interface of the four-way joint is communicated with the interior of the heating system through a hose.
Preferably, the heating system comprises a reaction cavity, an insulating layer and a thermocouple; the output end of the gas circuit system is communicated with the interior of the reaction cavity through a hose; heating wires are distributed in the reaction cavity; a thermocouple electrically connected with the heating wire is inserted into the reaction cavity; the bottom end of the thermocouple penetrates out of the reaction cavity, and a thermocouple joint is welded at the end part of the thermocouple; an electrode joint is arranged below the thermocouple joint; the electrode joint is electrically connected with the thermocouple joint through a lead; the upper end and the lower end of the reaction cavity are both provided with heat preservation layers fixed on the upper wall and the lower wall of the reaction cavity.
Preferably, an insulating interlayer is arranged between the reaction cavity and the heating wire, and the insulating interlayer is a ceramic interlayer or a quartz interlayer.
Preferably, the reaction cavity is made of 316L stainless steel with excellent performance and is resistant to pressure of 20 MPa.
Preferably, the water cooling system comprises a water cooling shell and a water cooling pipe; a water-cooling shell is sleeved outside the heating system; a water-cooling pipe is arranged in the water-cooling shell; and the water inlet end of the water-cooling pipe is connected to the water outlet end of a water pump in the cooling water tank.
Preferably, the light supply device comprises a light inlet screw rod, a light inlet window, a light outlet pressing sheet and a light outlet window; a light inlet screw rod is inserted into the middle of the heating system along the transverse direction; the light inlet screw is externally provided with threads, and a light inlet channel with one end communicated with the outside is formed in the light inlet screw along the axis direction; a light inlet window is fixed on the inner wall of the front end of the light inlet channel; along the central line of the light inlet channel, the sample cover is fixed at the front end of the light inlet window; the light outlet window is arranged at the front end of the light inlet window; and the light-emitting window is bonded on the heating system; a light outlet pressing sheet is fixed on the front side of the light outlet window; the front end of the light-emitting port pressing sheet is flared, the rear end of the light-emitting port pressing sheet is contracted, and the caliber of the light-emitting port pressing sheet is slightly larger than that of the light-entering window.
Preferably, the light exit window is a pressure-resistant window of phi 16x2mm, and the clear aperture of the light exit window is 5 mm; the light inlet window is a pressure-resistant window phi 8x2mm, and the clear aperture of the light inlet window is 4 mm.
Preferably, the light supply device further comprises a sealing assembly; the sealing assembly comprises a first sealing ring, a second sealing ring and a third sealing ring; the light inlet screw is sealed on the heating system through a first sealing ring; a second sealing ring is also arranged between the sample cover and the rod head of the light inlet screw; and a third sealing ring is also arranged between the light-emitting port pressing sheet and the heating system.
Preferably, the water cooling system and the heating system wrapped inside the water cooling system are both fixed on the base.
The light inlet screw is taken out from the reaction cavity in a counterclockwise rotating mode, the sample cover is taken down, the reaction sample is placed into the sample cavity in the sample cover, then the sample cover is covered on the light inlet screw, and the sample cover is screwed into the reaction cavity in the clockwise mode. And closing the first ball valve, opening an air source, introducing the MPa gas into the reaction cavity from the second ball valve through the pressurizing unit, wherein the pressure gauge can display the pressure, and when the pressure exceeds the maximum pressure by 20MPa, the excess gas exceeding the pressure can be discharged by the unloading valve. Then a water pump in the cooling water tank is opened, and the reaction cavity wrapped in the water-cooled shell is cooled through the water-cooled tube until the required temperature is reached; the device is mainly suitable for various conditions with high temperature and high pressure requirements, such as supercritical reaction, and realizes various spectroscopy structure characterizations under the conditions of high temperature and high pressure by matching different optical windows, namely different light-emitting windows and light-entering windows, such as X-ray absorption spectroscopy (sXAS), small angle X-ray scattering (SAXS), inelastic X-ray scattering (Rixs), Raman, infrared and the like. The structural analysis and study of solution systems under supercritical reaction conditions is ultimately achieved by using a combination of these various techniques on samples under extreme conditions. The use of XAS technology, for example, can provide information on the atomic scale around a particular atom, but SAXS is sensitive to the magnitude and amplitude of density fluctuations that occur in the liquid compressible state. RIXS refers to a variety of specific techniques, several of which are cited to enable measurement of dynamic structural factors to determine parameters of structural relaxation in hydrogen bonding liquids. The combination of infrared and Raman spectroscopy technologies can realize the relevant reaction kinetic information of molecular vibration of the liquid under the supercritical reaction condition, and provide the most basic structural information for researching the reaction kinetic mechanism of the substances under the conditions of high temperature and high pressure; and the water cooling system consists of a water cooling shell and a water cooling pipe, the whole body is connected by a PU hose, the surface temperature is less than 60 ℃, and the experimenters are protected from being scalded.
Compared with the prior art, the invention has the beneficial effects that:
A. the method is suitable for various conditions with high temperature and high pressure requirements, such as supercritical reaction, and realizes various spectroscopy structure characterizations under the conditions of high temperature and high pressure by matching different optical windows, namely different light-out windows and light-in windows, such as X-ray absorption spectroscopy (sXAS), small angle X-ray scattering (SAXS) and inelastic X-ray scattering (Rixs), Raman, infrared and the like. The structural analysis and study of solution systems under supercritical reaction conditions is ultimately achieved by using a combination of these various techniques on samples under extreme conditions. The use of XAS technology, for example, can provide information on the atomic scale around a particular atom, but SAXS is sensitive to the magnitude and amplitude of density fluctuations that occur in the liquid compressible state. RIXS refers to various specific technologies, and measurement of dynamic structural factors is realized by light introduction of a light supply device, temperature supply of a water cooling system and pressure control of a gas system, so as to determine structural relaxation parameters in hydrogen bond liquid. The combination of infrared and Raman spectroscopy technologies can realize the relevant reaction kinetic information of molecular vibration of the liquid under the supercritical reaction condition, provide the most basic structural information for researching the reaction kinetic mechanism of the substances under the conditions of high temperature and high pressure, reduce the influence of an external light source on the test by controlling light rays, and improve the test accuracy;
B. the water cooling system consists of a water cooling shell and a water cooling pipe, the whole body is connected by a PU hose, the surface temperature is less than 60 ℃, and experimenters are protected from being scalded.
Drawings
FIG. 1 is a schematic diagram of an overall front sectional structure of a supercritical in-situ spectroscopy reaction apparatus according to the present invention;
FIG. 2 is an enlarged view of the area A in FIG. 1 according to the present invention.
Description of the drawings: 1. a gas path system; 11. an unloading valve; 12. a first ball valve; 13. a tee joint; 14. a pressure gauge; 15. four-way connection; 16. a second ball valve; 2. a heating system; 21. a reaction chamber; 22. a heat-insulating layer; 23. a thermocouple; 24. a thermocouple junction; 25. an electrode tab; 3. a water cooling system; 31. water-cooling the housing; 32. a water-cooled tube; 4. a sample cover; 41. a sample chamber; 5. a light supply device; 51. a light inlet screw; 52. a seal assembly; 521. a first seal ring; 522. a second seal ring; 523. a third seal ring; 53. a light entrance window; 54. a light-emitting port pressing sheet; 55. a light exit window; 6. a base.
Detailed Description
In order to facilitate the understanding of the technical solutions of the present invention for those skilled in the art, the technical solutions of the present invention will be further described with reference to the drawings attached to the specification.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
Referring to fig. 1, the present embodiment discloses a supercritical in-situ spectrum reaction apparatus, which includes a gas path system 1, a heating system 2, a water cooling system 3, a reaction chamber 21, and a light supply device 5.
The gas path system 1 comprises an unloading valve 11, a first ball valve 12, a tee joint 13, a pressure gauge 14, a clamping sleeve 15 and a second ball valve 16. The unloading valve 11, the pressure gauge 14 and the second ball valve 16 are sequentially connected to the gas through pipe. The tee joint 13 is communicated with a branch pipe through a sleeve. A first ball valve 12 is mounted on the branch pipe. The pressure gauge 14 is connected to the gas pipe through a cross 15, but the connection mode of the gas system fittings is not limited to the single fixing mode, and the pressure can be detected by connecting various fittings and pressure testing devices in other various modes.
The heating system 2 comprises a reaction cavity 21, an insulating layer 22 and a thermocouple 23. The other interface of the four-way joint 15 is communicated with the interior of the reaction cavity 21 through a hose. Heating wires are distributed in the reaction cavity 21. An insulating interlayer is arranged between the reaction cavity 21 and the heating wire. The insulating interlayer is a ceramic interlayer or a quartz interlayer or other insulating layer materials with the same heat insulation effect. A thermocouple 23 electrically connected with the heating wire is inserted into the reaction cavity 21. The bottom end of the thermocouple 23 penetrates out of the reaction cavity 21, and the end part is welded with a thermocouple joint 24. An electrode joint 25 is arranged below the thermocouple joint 24. The electrode connector 25 and the thermocouple connector 24 are electrically connected through a lead. The upper end and the lower end of the reaction cavity 21 are both provided with heat preservation layers 22 adhered to the upper wall and the lower wall of the reaction cavity 21.
The water cooling system 3 comprises a water cooling shell 31 and a water cooling pipe 32. The reaction chamber 21 is externally sleeved with a water-cooling shell 31. A water cooling pipe 32 is arranged in the water cooling shell 31. The water inlet end of the water cooling pipe 32 is connected to the water outlet end of a water pump (not shown) stored in a cooling water tank (not shown).
Referring to fig. 1 and 2, the light supplying device 5 includes a light inlet screw 51, a sealing assembly 52, a light inlet window 53, a light outlet pressing sheet 54, and a light outlet window 55. A light inlet screw 51 is inserted into the middle of the reaction cavity 21 along the transverse direction. The light inlet screw rod 51 is externally threaded, and a light inlet channel with one end communicated with the outside is formed inside the light inlet screw rod 51 along the axial direction. And a light inlet window 53 is adhered to the inner wall of the front end of the light inlet channel. Along the central line of the light inlet channel, the front end of the light inlet window 53 is also adhered with a sample cover 4. The center of the sample cover 4 is further opened with a sample cavity 41 for placing a sample. The light exit window 55 is disposed at a front end of the light entrance window 53. And the light exit window 55 is adhered to the reaction chamber 21. A light emitting pressing sheet 54 is adhered to the front side of the light emitting window 55. The light-emitting port pressing sheet 54 has a flared front end and a narrowed rear end, and the aperture is slightly larger than that of the light-entering window 53. The window connection method is not limited to this fixing method, and may be fixed by a screw fixing method or the like.
The light-emitting window55 is phi 16x2mm Al2O3The plate or the diamond plate or other pressure-resistant materials with the same effect have the light-transmitting aperture of 5 mm. The light inlet window 53 is made of phi 8x2mm Al2O3The plate or the diamond plate or other pressure-resistant materials with the same effect have the clear aperture of 4 mm.
The reaction cavity 21 is made of 316L stainless steel with excellent performance and is pressure-resistant to 20 MPa.
The water-cooling shell 31 and the reaction cavity 21 wrapped inside the water-cooling shell 31 are fixed on the base 6 through bolts.
The seal assembly 52 includes a first seal ring 521, a second seal ring 522, and a third seal ring 523. The light inlet screw 51 is sealed on the reaction cavity 21 by a first sealing ring 521. A second sealing ring 522 is further arranged between the sample cover 4 and the rod head of the light inlet screw 51. A third sealing ring 523 is further disposed between the light-emitting tabletting 54 and the reaction cavity 21. The seal assembly 52 includes, but is not limited to, one of the above-described sealing means, and other sealing means may be employed. The sealing effect is improved.
The working principle of the embodiment is as follows: the light inlet screw 51 is rotated counterclockwise from the reaction cavity 21, the sample cover 4 is taken down, the reaction sample is put into the sample cavity 41 of the sample cover 4, and then the sample cover 4 is covered on the light inlet screw 51 and is screwed into the reaction cavity 21 clockwise. The first ball valve 12 is closed, the gas source is opened, 20MPa gas is introduced into the reaction cavity 21 from the second ball valve 16 through the pressurizing unit, wherein the pressure gauge 14 can display the pressure, and when the pressure exceeds the maximum pressure of 20MPa, the excess gas exceeding the pressure can be discharged through the unloading valve 11. Then, a water pump in the cooling water tank is opened, and the reaction cavity 21 wrapped in the water-cooled shell 31 is cooled through the water-cooled tube 32 until the required temperature is reached; the device is mainly suitable for various conditions with high temperature and high pressure requirements, such as supercritical reaction, and various spectroscopy structure characterizations under the conditions of high temperature and high pressure are realized by matching different optical windows, namely different light-emitting windows 55 and light-entering windows 53, such as X-ray absorption spectroscopy (sXAS), small-angle X-ray scattering (SAXS), inelastic X-ray scattering (Rixs), Raman, infrared and the like. The structural analysis and study of solution systems under supercritical reaction conditions is ultimately achieved by using a combination of these various techniques on samples under extreme conditions. The use of XAS technology, for example, can provide information on the atomic scale around a particular atom, but SAXS is sensitive to the magnitude and amplitude of density fluctuations that occur in the liquid compressible state. RIXS refers to a variety of specific techniques, several of which are cited to enable measurement of dynamic structural factors to determine parameters of structural relaxation in hydrogen bonding liquids. The combination of infrared and Raman spectroscopy technologies can realize the relevant reaction kinetic information of molecular vibration of the liquid under the supercritical reaction condition, and provide the most basic structural information for researching the reaction kinetic mechanism of the substances under the conditions of high temperature and high pressure; moreover, the water cooling system 3 consists of a water cooling shell 31 and a water cooling pipe 32, the whole body is connected by a PU hose, the surface temperature is less than 60 ℃, and the experimenters are protected from being scalded.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The above-mentioned embodiments only represent embodiments of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the concept of the present invention, and these embodiments are all within the protection scope of the present invention.
Claims (10)
1. Supercritical in-situ spectrum reaction device, its characterized in that: comprises a gas path system, a heating system, a water cooling system, a sample cover and a light supply device; the outside of the heating system is wrapped with a water cooling system for cooling the heating system; the interior of the heating system is communicated with the gas output end of the gas path system, and the gas path system provides required test pressure for the heating system through gas pressure; the light supply device penetrates through a heating area of the heating system; the sample cover is fixed at the front end of the light supply device for providing light sources with different spectrums; the center of the sample cover is provided with a sample cavity for placing a sample.
2. The supercritical in-situ spectroscopy apparatus of claim 1, wherein: the gas path system comprises an unloading valve, a first ball valve, a tee joint, a pressure gauge, a clamping sleeve and a second ball valve; the unloading valve, the pressure gauge and the second ball valve are sequentially connected to the gas through pipe; the tee joint is communicated with a branch pipe through a sleeve; the branch pipe is provided with a first ball valve; the pressure gauge is connected to the gas through pipe through a four-way joint; the other interface of the four-way joint is communicated with the interior of the heating system through a hose.
3. The supercritical in-situ spectroscopy apparatus of claim 1, wherein: the heating system comprises a reaction cavity, a heat insulation layer and a thermocouple; the output end of the gas circuit system is communicated with the interior of the reaction cavity through a hose; heating wires are distributed in the reaction cavity; a thermocouple electrically connected with the heating wire is inserted into the reaction cavity; the bottom end of the thermocouple penetrates out of the reaction cavity, and a thermocouple joint is welded at the end part of the thermocouple; an electrode joint is arranged below the thermocouple joint; the electrode joint is electrically connected with the thermocouple joint through a lead; the upper end and the lower end of the reaction cavity are both provided with heat preservation layers fixed on the upper wall and the lower wall of the reaction cavity.
4. The supercritical in-situ spectroscopy apparatus of claim 3, wherein: an insulating interlayer is arranged between the reaction cavity and the heating wire and is a ceramic interlayer or a quartz interlayer.
5. The supercritical in-situ spectroscopy apparatus of claim 3, wherein: the reaction cavity is made of 316L stainless steel with excellent performance and is resistant to pressure of 20 MPa.
6. The supercritical in-situ spectroscopy apparatus of claim 1, wherein: the water cooling system comprises a water cooling shell and a water cooling pipe; a water-cooling shell is sleeved outside the heating system; a water-cooling pipe is arranged in the water-cooling shell; and the water inlet end of the water-cooling pipe is connected to the water outlet end of a water pump in the cooling water tank.
7. The supercritical in-situ spectroscopy apparatus of claim 1, wherein: the light supply device comprises a light inlet screw rod, a light inlet window, a light outlet pressing sheet and a light outlet window; a light inlet screw rod is inserted into the middle of the heating system along the transverse direction; the light inlet screw is externally provided with threads, and a light inlet channel with one end communicated with the outside is formed in the light inlet screw along the axis direction; a light inlet window is fixed on the inner wall of the front end of the light inlet channel; along the central line of the light inlet channel, the sample cover is fixed at the front end of the light inlet window; the light outlet window is arranged at the front end of the light inlet window; and the light-emitting window is bonded on the heating system; a light outlet pressing sheet is fixed on the front side of the light outlet window; the front end of the light-emitting port pressing sheet is flared, the rear end of the light-emitting port pressing sheet is contracted, and the caliber of the light-emitting port pressing sheet is slightly larger than that of the light-entering window.
8. The supercritical in-situ spectroscopy apparatus of claim 7, wherein: the light-emitting window is a pressure-resistant window made of phi 16x2mm Al2O3 sheets or diamond sheets, and the clear aperture of the light-emitting window is 5 mm; the light inlet window is a pressure-resistant window made of phi 8x2mm Al2O3 sheets or diamond sheets, and the clear aperture of the light inlet window is 4 mm.
9. The supercritical in-situ spectroscopy apparatus of claim 7, wherein: the light supply device further comprises a sealing component; the sealing assembly comprises a first sealing ring, a second sealing ring and a third sealing ring; the light inlet screw is sealed on the heating system through a first sealing ring; a second sealing ring is also arranged between the sample cover and the rod head of the light inlet screw; and a third sealing ring is also arranged between the light-emitting port pressing sheet and the heating system.
10. The supercritical in-situ spectroscopy apparatus of claim 1, wherein: and the water cooling system and the heating system wrapped in the water cooling system are fixed on the base.
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|---|---|
| CN112730238B (en) | 2023-04-28 |
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