A multifunctional in-situ reaction device, reaction system and application
By designing a multifunctional in-situ reaction device and system, in-situ spectroscopy detection of the reaction processes of hydrothermal and molten salt methods is realized, the problem of lack of a systematic research platform in the existing technology is solved, high-performance research methods are provided, and the analysis ability of metastable phases is enhanced.
Patent Information
- Application Number
- CN202210755210.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-30
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2042-06-30
AI Technical Summary
The existing technology lacks a systematic and multi-directional research platform, and it is difficult to observe the kinetic/thermodynamic mechanisms of hydrothermal and molten salt methods during the reaction process through in-situ spectroscopy, especially the study of metastable phases.
A multifunctional in-situ reaction device and system is designed, including a reaction vessel, a pressure holder and an external heating system, which supports in-situ analysis of neutron spectroscopy, Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy. Reaction vessels of different materials are used to adapt to different spectral detection, and combined with magnetic stirring devices, real-time detection of the reaction process is achieved.
It provides a multifunctional and high-performance research platform that can accurately observe and analyze the kinetic/thermodynamic processes and mechanisms of hydrothermal and molten salt methods, improves the depth and comprehensiveness of the metastable phase, eliminates the interference of thermal expansion and contraction of the reaction vessel, and enhances the accuracy of spectral detection.
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Abstract
Description
Technical Field
[0001] The present invention relates to a chemical reaction device and system, and particularly to a multifunctional in-situ reaction device, reaction system and its application, which can be used for in-situ analysis of neutron reactors, Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy; it belongs to the experimental platform for chemical reaction mechanisms. Background Art
[0002] Spectral detection technology is the "super microscope" in the field of characterization science. Among a series of spectra, since neutrons are electrically neutral, have a magnetic moment, strong penetration power, can distinguish light elements, isotopes and neighboring elements, and can also be used to study the microscopic structure and motion laws of various substances at the atomic and molecular scales, it has made significant contributions to the research in many fields such as physics, chemistry, biology, materials and energy science. It can be widely applied to many disciplines such as basic scientific research and application technology promotion, and is one of the ideal tools for studying the microscopic structure and dynamic processes of substances.
[0003] Soft chemistry is a method for preparing materials through general chemical reactions at medium or low temperatures or in solutions, which was proposed by German solid chemist Schaefer in the early 1970s. Compared with hard chemistry carried out under extreme conditions such as ultra-high pressure, ultra-high temperature, ultra-high vacuum, strong radiation, and zero gravity, soft chemistry does not require extremely harsh conditions, can realize the chemical reaction process under mild conditions, and is easy to observe and control its chemical reaction process, path and mechanism, specifically including precursor method, hydrothermal method, sol-gel method, molten salt method reaction, etc. The products obtained by high-temperature solid-phase chemical reaction synthesis are thermodynamically stable, and under high-temperature and high-pressure conditions, the reaction process is relatively fast and it is difficult to perform in-situ tracking. And some metastable / metastable intermediate or kinetically controlled compounds are easy to decompose or recombine into thermodynamically stable products at high temperatures.
[0004] In order to deeply explore the mechanism of the reaction process, improve its kinetic process, and extract metastable / metastable phase intermediate products, it is necessary to lower the solid-phase reaction temperature and adopt a soft chemical synthesis method with mild reaction conditions. Among them, the molten salt method and the hydrothermal method are relatively widely used synthesis means in soft chemical synthesis. The hydrothermal method refers to a reaction carried out in a closed reaction kettle with water as the solvent, where the reactants react to form products under the autogenous pressure of water at a certain temperature. In the hydrothermal method, water is both a medium for transmitting pressure and a solvent for the reactants. The molten salt method refers to using one or several low-melting salts as the reaction medium. After mixing the salt and the reactants in a certain proportion and heating to melt the salt, the reactants react in the molten salt. After the reaction is completed, it is cooled to room temperature and then a suitable solvent is used to dissolve the salt. The synthetic product can be obtained after filtration and washing. Through these synthetic methods, it is possible to change its chemical composition, surface / crystal / molecular structure, morphology, multiphase / multilayer / composite structure, or provide strange chemical and physical properties, explore reaction mechanisms different from traditional materials, and thus break through the limitations of traditional materials.
[0005] In summary, the hydrothermal method and the molten salt method are crucial for the research and development of new energy storage materials and reaction mechanisms. However, most of the relevant literature focuses on ex-situ phase studies and lacks a systematic theory. It is necessary to develop a multi-faceted and high-performance comprehensive research platform to facilitate the observation of the kinetic / thermodynamic mechanisms of the hydrothermal method and the molten salt method during the reaction process through in-situ spectroscopic techniques. Summary of the Invention
[0006] To solve the deficiencies of the prior art, the purpose of the present invention is to provide a multifunctional in-situ reaction device and reaction system to facilitate in-depth and comprehensive research on the physical and chemical properties of metastable phases in soft chemical reactions and provide a reliable way to understand their kinetic processes and mechanisms.
[0007] To achieve the above objectives, the present invention adopts the following technical solutions:
[0008] The present invention first discloses a multifunctional in-situ reaction device, including: a reaction vessel, and a pressure maintainer for accommodating and locking the reaction vessel. The pressure maintainer includes a main body and a cover body that are detachably connected. The main body accommodates the reaction vessel therein and forms a blank window that exposes the reaction vessel for spectral penetration.
[0009] Preferably, the aforementioned spectrum is one of X-ray, neutron spectrum, Fourier transform infrared spectrum, Raman spectrum, or ultraviolet-visible spectrum. When different spectra are used as detection means, reaction vessels made of appropriate materials are correspondingly used to achieve multi-functional and multi-occasion applications.
[0010] Preferably, when neutron spectroscopy is adopted, the aforementioned reaction vessel is made of a material transparent to neutrons, and specifically, it can be selected from a vanadium metal vessel, a fused silica vessel, a titanium-zirconium neutron-transparent matrix alloy vessel, and a polyether ether ketone polymer vessel.
[0011] More preferably, the aforementioned pressure retainer is made of stainless steel material or polyether ether ketone polymer material, which can ensure reliable mechanical properties of the pressure retainer. Moreover, the polyether ether ketone polymer material has a low absorption rate of X-rays and neutrons. The retainer made of it has good hardness and strength and is the first choice for X-ray and neutron spectroscopy detection.
[0012] More preferably, the aforementioned main body and the cover are detachably connected by means of threads or snaps. The cover includes a connecting portion and a locking portion. A plurality of mounting slots are formed on the outer peripheral wall of the top of the connecting portion.
[0013] Further preferably, the aforementioned main body includes an upper limiting structure, a lower limiting structure, and a longitudinal connecting rod for connecting the two. The blank area between the upper limiting structure and the lower limiting structure except for the longitudinal connecting rod forms an integral blank window. By adopting a large-area arc-shaped window and cooperating with the reaction vessel with a rotary body structure, the background interference generated by multiple scattering spectra can be prevented, thereby improving the accuracy of the spatial resolution small-angle spectral scattering test.
[0014] Further preferably, both the aforementioned upper limiting structure and the lower limiting structure have a central through cavity. An adjusting piece is arranged at the top of the upper limiting structure to close the top opening of the upper limiting structure and play a role in adjusting the height and pressure of the reaction vessel.
[0015] Even more preferably, a stepped hole is arranged in the aforementioned lower limiting structure, and a balancing piece is arranged at the stepped hole. The reaction vessel is limited between the adjusting piece and the balancing piece. This balancing piece can not only play an effective supporting role but also protect the reaction vessel, make the bottom of the reaction vessel stress balanced, and eliminate the interference caused by thermal expansion and contraction.
[0016] Still further preferably, the aforementioned longitudinal connecting rod, upper limiting structure, and lower limiting structure are integrally formed.
[0017] Even more preferably, at least one positioning groove is formed on the outer peripheral wall of the bottom of the aforementioned lower limiting structure, which cooperates with the aforementioned mounting slots mentioned above. The upper and lower positioning makes the reactor more stably installed on the detection platform at high temperatures.
[0018] Even more preferably, the aforementioned cover, upper limiting structure, lower limiting structure, adjusting piece, and balancing piece are rotary body components arranged coaxially.
[0019] Still further preferably, a handle is further provided on the cover body, and a through hole is formed at the top of the handle. By inserting a tool into the through hole and applying an external force, the cover body can be locked or loosened.
[0020] The present invention also discloses a multifunctional in-situ reaction system, including an external heating system and a multifunctional in-situ reaction device as described above.
[0021] Preferably, the multifunctional in-situ reaction system further includes a magnetic stirring device.
[0022] The present invention also discloses the application of the multifunctional in-situ reaction system as described above in an in-situ hydrothermal reactor and an in-situ molten salt reactor.
[0023] In addition, the present invention also discloses a method for realizing in-situ detection by using the system as described above, including the following steps:
[0024] (1) Adding reactants into a reaction vessel and sealing the reaction vessel;
[0025] (2) Placing the reaction vessel in the main body of a pressure maintainer, adjusting and installing the adjusting piece and the balancing piece, and connecting the cover body to the main body to lock the reaction vessel;
[0026] (3) Fixing the connected in-situ reaction device to a detection platform and heating it in an external heating system;
[0027] (4) Starting the reaction system, and simultaneously performing real-time detection on the sample in the reaction vessel through spectroscopy to realize in-situ characterization of the sample reaction process.
[0028] The advantages of the present invention are as follows:
[0029] (1) The reaction device and system of the present invention are simple, compact and ingenious in structure. The pressure maintainer accommodates and locks the reaction vessel therein. The adjusting piece and the balancing piece respectively arranged at the top and bottom of the pressure maintainer can not only protect the reaction vessel, but also eliminate the interference caused by the thermal expansion and contraction of the reaction vessel that may occur during the reaction process, ensuring the accuracy of the obtained experimental data;
[0030] (2) The device is not only applicable to neutron spectroscopy analysis, but also applicable to in-situ analysis of Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy, providing a multi-spectral analysis method for understanding and exploring the kinetic / thermodynamic processes and mechanisms of the hydrothermal method and the molten salt method, providing a multifunctional and high-performance research platform for users, enriching the characterization means of energy storage materials, helping to promote energy storage material scientists to more deeply and comprehensively study the physical and chemical properties of metastable phases in the hydrothermal method and the molten salt method, and providing a reliable way to understand their kinetic processes and mechanisms;
[0031] (3) The reaction container of the device can be a vanadium metal container, a fused quartz container, a titanium-zirconium neutron-transparent matrix alloy container, a polyetheretherketone polymer container, etc., which are transparent to neutrons and do not absorb neutrons (other materials absorb neutrons and affect the test signal). It can truly reflect the structure and performance of the material in situ. The sample can be crystallized and synthesized in situ under high temperature conditions, and can provide an in-situ reaction platform for performance testing of solutions, battery films and other materials;
[0032] (4) The device can be stably installed on the detection platform through the design of upper and lower clamps to ensure the stability of the reaction container. The blank window is designed as an integral arc-shaped large-area window, and the reaction container is correspondingly designed as a rotating body structure, which can improve the accuracy of spatially resolved small-angle spectral scattering tests and prevent background interference caused by multiple scattering spectra. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 It is a structural schematic diagram of a multifunctional in-situ reaction device of the present invention;
[0034] Figure 2 yes Figure 1 A schematic diagram of the structure of the embodiment shown after the reaction vessel is removed;
[0035] Figure 3 yes Figure 2 Schematic diagram of the cross-section structure;
[0036] Figure 4 yes Figure 2 A schematic structural diagram of the cover body;
[0037] Figure 5 yes Figure 2 Schematic diagram of the structure of the balance piece.
[0038] The meanings of the reference numerals in the figure are: 1. reaction vessel, 2. pressure retainer, 3. main body, 4. cover body, 301. upper limit structure, 302. lower limit structure, 303. longitudinal connecting rod, 401. connecting part, 402. locking part, 403. through hole, 5. adjusting plate, 6. balancing plate, 7. mounting slot, 8. positioning slot. DETAILED DESCRIPTION
[0039] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
[0040] In the description of the present invention, it should be understood that the orientation or positional relationships indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. are based on the orientation or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance.
[0041] Embodiment 1
[0042] The structure of the multifunctional in-situ reaction device of this embodiment is as Figure 1 shown, and it includes: a reaction vessel 1 and a pressure retainer 2. Among them, the pressure retainer 2 is used to accommodate and lock the reaction vessel 1. In order to endow the pressure retainer 2 with reliable mechanical properties, it is entirely made of stainless steel material or polyether ether ketone polymer material. In addition, considering that the polyether ether ketone polymer material has a low absorption rate of X-rays and neutrons, the holder made of it has good hardness and strength, and is the preferred material for X-ray and neutron spectroscopy detection.
[0043] In order to achieve in-situ detection, a blank window is formed on the pressure retainer 2 for exposing a part of the reaction vessel 1 for spectrum penetration. In this embodiment, the pressure retainer 2 specifically includes a main body 3 and a cover 4 that are detachably connected, and the two are detachably connected by a threaded method. In practical applications, a snap connection method can also be selected according to needs.
[0044] Among them, the structure of the main body 3 is as Figure 2 and Figure 3 shown, and it includes: an integrally formed upper limit structure 301, a lower limit structure 302, and a longitudinal connecting rod 303 (only one) for connecting the two. The blank area between the upper limit structure 301 and the lower limit structure 302 except the longitudinal connecting rod 303 constitutes an overall blank window. By adopting this large-area arc-shaped window opening and cooperating with the reaction vessel 1 with a rotary body structure, the background interference generated by multiple scattered spectra can be avoided, and the accuracy of small-angle spectral scattering test with high spatial resolution can be significantly improved.
[0045] The structure of the cover 4 is as Figure 4As shown, the cover 4 comprises a connecting portion 401 and a locking portion 402. The upper limit structure 301 described above cooperates with the connecting portion 401. By adjusting the depth of the thread rotation, the height of the in-situ reaction device can be controlled, making it suitable for testing platforms of various specifications and models. The locking portion 402 of the cover 4 is also provided with a handle. A through-hole 403 is formed at the top of the handle. Inserting a tool into the through-hole 403 and applying external force can tighten or loosen the cover 4.
[0046] As a further improvement of this embodiment, both the upper limit structure 301 and the lower limit structure 302 have a central through cavity, and as shown in FIG. Figure 3 As shown, an adjusting piece 5 is provided on the top of the upper limit structure 301, a step hole is provided in the lower limit structure 302, and a balancing piece 6 (its structure is shown in FIG. Figure 5 As shown in the figure, after the reaction apparatus is assembled, the reaction vessel 1 is confined between the adjusting piece 5 and the balancing piece 6. The adjusting piece 5 closes the top opening of the upper limit structure 301 and serves to adjust the height and control the pressure of the reaction vessel 1. The balancing piece 6 not only provides effective support but also protects the reaction vessel 1, ensuring balanced force on the bottom of the reaction vessel 1. The adjustment piece 5 and the balancing piece 6 work together to eliminate interference caused by thermal expansion and contraction of the reaction vessel 1, thereby ensuring the service life of the reaction vessel 1.
[0047] This reaction device is multifunctional because its detection spectrum can be selected from neutron spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, or ultraviolet-visible spectroscopy. When using different spectral detection methods, the reaction vessel 1 can be replaced with a different material accordingly, achieving multifunctional and multi-purpose applications. When using neutron spectroscopy, the reaction vessel 1 is made of a neutron-transparent material, specifically a vanadium metal container, a fused silica container, a titanium-zirconium neutron-transparent matrix alloy container, or a polyetheretherketone polymer container.
[0048] In order to quickly install the reaction device, several installation slots 7 are formed on the top outer wall of the connecting part 401, and at least one positioning slot 8 is formed on the bottom outer wall of the lower limit structure 302. The upper and lower positioning structural design enables the reaction container 1 to be more stably installed on the detection platform.
[0049] In this embodiment, the cover 4, the upper limit structure 301, the lower limit structure 302, the adjustment plate 5 and the balance plate 6 are coaxially arranged rotating parts. In this way, the reaction vessel 1 installed therein is also a rotating structure, which is not only convenient for installation but also can effectively avoid the background interference caused by multiple scattering spectra, and significantly improve the accuracy of spatially resolved small-angle spectral scattering tests.
[0050] Example 2
[0051] In this embodiment, the number of the longitudinal connecting rods 303 is set to be 2 to 4. It has been verified that the accuracy rate of the obtained detection results is greatly reduced. The applicant analyzed that this may be because the 2 to 4 longitudinal connecting rods 303 divide the blank window in Embodiment 1 into multiple small windows, thus affecting the detection results.
[0052] Embodiment 3
[0053] This embodiment discloses a multifunctional in-situ reaction system, including an external heating system, and also including the multifunctional in-situ reaction device as in Embodiment 1.
[0054] Embodiment 4
[0055] The multifunctional in-situ reaction system of this embodiment further includes a magnetic stirring device, and during the use process, the magnetic stirring equipment can be selected to be loaded or not loaded according to needs, and homogeneous or heterogeneous reactions can be realized.
[0056] Embodiment 5
[0057] This embodiment discloses the application of a multifunctional in-situ reaction system as described in Embodiment 3 or 4 in the in-situ hydrothermal method. The steps are as follows:
[0058] (1) Add the reactants into the reaction vessel 1 and seal the reaction vessel 1;
[0059] (2) Place the reaction vessel 1 into the main body 3 of the pressure maintainer 2, adjust and install the adjusting piece 5 and the balancing piece 6, and connect the cover body 4 to the main body 3 to lock the reaction vessel 1;
[0060] (3) Fix the connected in-situ reaction device to the detection platform and place it in the external heating system for heating;
[0061] (4) Start the reaction system, and at the same time, perform real-time detection on the sample in the reaction vessel 1 through spectroscopy to realize the in-situ characterization of the sample reaction process.
[0062] The specific application process is as follows: Using heavy water (D2O) as the reaction solution, with a maximum capacity of 50% of the container and a maximum use temperature of 250 °C. The precursor can be metal oxides, nitrates, sulfates, chlorides, acetates, silicates, fluorides, phosphates, carbonates, metals; the concentration should be controlled between 0 and 10 moles, the reaction time should be controlled within 100 days, and the pH value should be controlled between 1 and 14.
[0063] The precursor should be placed in a vanadium metal container / fused silica container / titanium-zirconium neutron-transparent matrix alloy container / polyetheretherketone polymer reaction vessel 1, an appropriate amount of solution should be added, and then the reaction vessel 1 should be closed; then the reaction vessel 1 should be placed in a pressure maintainer 2 and locked, and finally placed in an external heating system for heating. During the heating process, in-situ testing of the reaction process is carried out by neutron spectroscopy / Fourier transform infrared spectroscopy / ultraviolet-visible spectroscopy.
[0064] Example 6
[0065] This example discloses the application of a multifunctional in-situ reaction system as described in Example 3 or 4 in the in-situ molten salt method.
[0066] The specific application process is as follows: A single salt or a mixed salt is used as the reaction medium, and the salts can be metal nitrates, metal sulfates, metal chlorides, or metal fluorides. The maximum capacity is 50% of the container, and the maximum operating temperature is 950 °C. The precursor can be a metal oxide, nitrate, sulfate, chloride, acetate, silicate, fluoride, phosphate, carbonate, or metal; the concentration should be controlled between 0 and 10 moles, the reaction time should be controlled within 100 days, and the pH value should be controlled between 1 and 14.
[0067] The precursor should be placed in a vanadium metal container / fused silica container / titanium-zirconium neutron-transparent matrix alloy container / polyetheretherketone polymer reaction vessel 1, an appropriate amount of solution should be added, and then the reaction vessel 1 should be closed; then the reaction vessel 1 should be placed in a pressure maintainer 2 and locked, and finally placed in an external heating system for heating. During the heating process, in-situ testing of the reaction process is carried out by neutron spectroscopy / Fourier transform infrared spectroscopy / ultraviolet-visible spectroscopy.
[0068] In summary, the reaction device and system of the present invention are compact and ingenious in structure. The pressure maintainer 2 accommodates and locks the reaction vessel 1 therein. The adjusting piece 5 and the balancing piece 6 respectively arranged at the top and bottom of the pressure maintainer 2 can not only protect the reaction vessel 1, but also eliminate the interference caused by thermal expansion and contraction that may occur during the reaction process, ensuring the accuracy of the experimental data obtained; at the same time, the device is not only applicable to neutron spectroscopy analysis, but also applicable to in-situ analysis of Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy, providing a multi-spectral analysis method for understanding and exploring the kinetic / thermodynamic processes and mechanisms of the hydrothermal method and the molten salt method, providing a multifunctional and high-performance research platform for users, enriching the characterization means of energy storage materials, and helping to promote more in-depth and comprehensive research on the physical and chemical properties of metastable phases in the hydrothermal method and the molten salt method by energy storage material scientists, and providing a reliable way to understand their kinetic processes and mechanisms.
[0069] In the description of the present invention, it should be noted that unless otherwise clearly specified and defined, the terms "installed", "connected", and "coupled" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.
[0070] In the description of this specification, the description referring to terms such as "one embodiment", "some embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.
[0071] The above shows and describes the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the above embodiments do not limit the present invention in any form. Any technical solutions obtained by using equivalent replacements or equivalent transformations fall within the protection scope of the present invention.
Claims
1. A multifunctional in-situ reaction device, characterized in that, Comprising: A reaction vessel, a pressure maintainer for accommodating and locking the reaction vessel, the pressure maintainer including a main body and a cover detachably connected, the main body accommodating the reaction vessel therein and having a blank window formed thereon for exposing a part of the reaction vessel for spectral penetration; The main body includes: an upper limit structure, a lower limit structure, and a longitudinal connecting rod for connecting the two, and the blank area between the upper limit structure and the lower limit structure except for the longitudinal connecting rod constitutes an integral blank window; Both the upper limit structure and the lower limit structure have a central through cavity, and an adjusting piece is provided at the top of the upper limit structure, and the adjusting piece is used to close the top opening of the upper limit structure to adjust the height and pressure of the reaction vessel; A stepped hole is provided in the lower limit structure, and a balancing piece is provided at the stepped hole, and the balancing piece is used to support and protect the reaction vessel, and the reaction vessel is limited between the adjusting piece and the balancing piece; The longitudinal connecting rod, the upper limit structure, and the lower limit structure are integrally formed; The cover, the upper limit structure, the lower limit structure, the adjusting piece, and the balancing piece are rotary body components coaxially arranged.
2. The multifunctional in-situ reaction device according to claim 1, wherein The spectrum is one of X-ray, neutron spectrum, Fourier transform infrared spectrum, Raman spectrum, or ultraviolet-visible spectrum.
3. The multifunctional in-situ reaction device according to claim 2, characterized in that, The spectrum is a neutron spectrum, and the reaction vessel is selected from one of a vanadium metal container, a fused silica container, a titanium zirconium neutron-transparent matrix alloy container, or a polyetheretherketone polymer container.
4. The multifunctional in-situ reaction device according to claim 3, characterized in that, The pressure maintainer is made of stainless steel material or polyetheretherketone polymer material.
5. A multifunctional in-situ reaction device according to claim 1, characterized in that, The main body and the cover are connected by a threaded or snap-fastening method, and the cover includes a connecting portion and a locking portion.
6. The multifunctional in-situ reaction device according to claim 5, characterized in that, A handle is provided on the locking portion of the cover, and a through hole is formed on the handle.
7. A multifunctional in-situ reaction device according to claim 5, characterized in that, A plurality of mounting slots are formed on the outer peripheral wall of the top of the connecting portion.
8. A multifunctional in-situ reaction device according to claim 1, characterized in that At least one positioning groove is formed on the outer peripheral wall of the bottom of the lower limit structure.
9. A multifunctional in-situ reaction system, characterized in that, Comprising an external heating system, and also comprising a multifunctional in-situ reaction device according to any one of claims 1 to 8.
10. A multifunctional in-situ reaction system according to claim 9, characterized in that, Also comprising a magnetic stirring device.
11. Application of a multifunctional in-situ reaction system according to claim 9 in an in-situ hydrothermal reactor and an in-situ molten salt reactor.
12. A method for realizing in-situ detection by using the system according to claim 9, comprising the following steps: (1) Adding a reaction precursor and a solution into the reaction vessel and sealing the reaction vessel; (2) Placing the reaction vessel into the main body of the pressure maintainer, adjusting and installing the adjusting piece and the balancing piece, and connecting the cover to the main body to lock the reaction vessel; (3) Fixing the connected in-situ reaction device to a detection platform and heating it in an external heating system; (4) Starting the reaction system, and simultaneously performing real-time detection on the sample in the reaction vessel through a spectrum to realize in-situ detection of the sample reaction process.
Citation Information
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In-situ reaction device and optical in-situ reaction characterization system and method
CN110361350A