An in-situ photocatalytic nuclear magnetic detection device

Abstract

An embodiment of the present invention provides an in-situ photocatalytic nuclear magnetic detection device, including: a fiber optic collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe, which is used for in-situ photocatalytic reaction and receiving the nuclear magnetic signals of compounds during the reaction process. The fiber optic component in the nuclear magnetic resonance probe is connected to an external laser and extends into the interior of the nuclear magnetic resonance probe to introduce laser light into the interior of the nuclear magnetic resonance probe. The optical mirror component in the nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for converging, collimating and adjusting the direction of the laser light emitted by the fiber optic component. The ferrule component in the nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for supporting and limiting the fiber optic component and the optical mirror component; a magnet, a cabinet and a nuclear magnetic signal real-time acquisition system: which are matched with the nuclear magnetic resonance probe to obtain the nuclear magnetic signals of compounds in the reaction system during the photocatalytic process.

Description

Technical Field

[0001] The embodiments of the present invention relate to the field of in-situ detection of nuclear magnetic signals, and particularly to an in-situ photocatalytic nuclear magnetic detection device. Background Technique

[0002] Photocatalytic reaction is a process that utilizes light energy to excite semiconductor materials to generate electron-hole pairs, thereby driving redox reactions. Due to its efficient and environmentally friendly characteristics, this technology exhibits great application potential in fields such as environmental purification and energy conversion. However, to improve photocatalytic efficiency and gain a deeper understanding of its mechanism, it is necessary to monitor and analyze the active species and intermediate products during the reaction process in real time and accurately.

[0003] In-situ nuclear magnetic resonance technology (In situ Nuclear Magnetic Resonance, NMR), as a non-destructive and highly sensitive analytical method, can monitor the chemical changes during the photocatalytic process in real time without interfering with the reaction. Through in-situ NMR signal detection, researchers can obtain information on various aspects such as the photocatalytic reaction mechanism, the generation and consumption of active species, and the adsorption situation on the catalyst surface.

[0004] In photocatalytic reactions, in-situ NMR technology is mainly applied in the following aspects:

[0005] Detection and identification of active species: During the photocatalytic process, the generation and recombination of electron-hole pairs are key steps. Through in-situ NMR technology, the generation and consumption processes of these active species can be directly observed, thereby revealing their action mechanisms in the photocatalytic reaction.

[0006] Analysis of reaction mechanism: The mechanism of photocatalytic reaction is complex, involving multiple intermediate products and side reactions. In-situ NMR technology can track the dynamic changes of specific atoms or functional groups, providing important clues for revealing the reaction pathway and mechanism.

[0007] Evaluation of catalyst performance: By monitoring the changes in NMR signals during the photocatalytic reaction process, performance indicators such as the activity, stability, and selectivity of the catalyst can be evaluated, providing a basis for the optimization and improvement of the catalyst.

[0008] Precisely because in-situ nuclear magnetic signal detection technology plays an increasingly important role in the research of photocatalytic reactions, and currently many of the photocatalytic devices of existing nuclear magnetic spectrometers are built by users themselves and do not possess characteristics such as high power, high stability, and convenient wavelength selection. It is necessary to design a simple, efficient, and easy-to-use in-situ NMR to deeply study the reaction mechanism of photocatalysis.

[0009] In addition, due to the wide variety, complex structure, and narrow internal space of commercial NMR probes, optical components cannot be directly placed in the probes, and in-situ photocatalysis of samples cannot be carried out in the probes. Most of the existing in-situ photocatalytic nuclear magnetic resonance detections focus on the modification of NMR tubes, that is, introducing optical fibers and LEDs into the NMR tubes and designing a matching NMR cap. This method has a simple light source device, low cost, is not limited by the magnet model, and does not require probe modification. However, there are problems such as low light intensity, uneven light illumination, and troublesome sample injection and extraction, which affect the photocatalytic effect. Summary of the Invention

[0010] To solve the above technical problems, the present invention provides an optical fiber collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe and its detection device:

[0011] First, select a dual-resonance micro broadband probe with a large internal modification design space. Its transmit / receive coil has a relatively small volume and occupies less space, providing sufficient space for embedding optical components inside the probe. Secondly, in the optical path design inside the probe, select the "collimating and reflecting" scheme instead of the "direct-incidence and diverging" scheme. The "direct-incidence and diverging" scheme is to introduce an optical fiber directly below the sample to irradiate the sample. Since the temperature control heating wire of the probe is also located directly below the probe, this scheme will damage the variable temperature function of the probe and there are also problems such as low light intensity and uneven light illumination, which affect the photocatalytic effect. The "collimating and reflecting" scheme is to design an optical path independent of the key components of the probe such as the tuning bar, temperature control device, capacitor, transmit / receive coil, etc. at the edge position inside the probe and can accommodate a 2mm optical fiber. One end of the optical fiber is connected to a laser, and the other end passes through the bottom of the probe, passes through the newly designed bypass at the internal edge of the probe, and is finally connected to a ferrule assembly that matches the structure of the NMR probe base. There is no need to drill holes and it will not damage the key components of the probe. The light source input into the probe is radiated by the angular mirror embedded in the ferrule assembly, passes through the gap of the RF coil, irradiates the sample in the NMR tube, and then triggers a photocatalytic reaction. Finally, place the probe in a high-field magnet and combine it with a cabinet, a data acquisition system, etc. to monitor the progress of the photocatalytic reaction in real time and conduct efficient research on the photocatalytic reaction mechanism and kinetics under in-situ conditions.

[0012] All in all, this application designs a "collimating and reflecting" light source input system for the probe, introducing an independent "collimating and reflecting" light source input system, enabling it to not only retain the original functions but also have the ability to carry out in-situ photocatalytic reactions and detect the nuclear magnetic signals of photocatalytic products.

[0013] Specifically, the entire set of in-situ photocatalytic nuclear magnetic resonance detection device includes:

[0014] Fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe, which is used for in-situ photocatalytic reaction and receiving nuclear magnetic signals of compounds during the reaction process. The fiber optic component in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe is connected to an external laser and extends into the nuclear magnetic resonance probe to introduce laser into the nuclear magnetic resonance probe. The optical mirror component in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for converging, collimating and adjusting the direction of the laser emitted by the fiber optic component. The ferrule component in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for supporting and limiting the fiber optic component and the optical mirror component; a laser, which is used to provide the light source required for the photocatalytic reaction;

[0015] Magnet, cabinet and nuclear magnetic signal real-time acquisition system: matching with the nuclear magnetic resonance probe to obtain the nuclear magnetic signals of the reaction system during the photocatalytic process.

[0016] In some embodiments, the optical path design inside the nuclear magnetic resonance probe adopts a collimating reflective scheme, including designing an optical path independent of the key components of the probe such as the tuning bar, temperature control device, capacitor, and transmit / receive coil at the edge position inside the nuclear magnetic resonance probe and capable of accommodating a 2-mm fiber optic. One end of the fiber optic is connected to the laser, and the other end passes through the bottom of the nuclear magnetic resonance probe and passes through the newly designed bypass inside the nuclear magnetic resonance probe, and finally is connected to the ferrule component that matches the main structure of the nuclear magnetic resonance probe. The light source input into the probe is reflected by the corner mirror embedded in the ferrule component, passes through the gap of the radio frequency coil, and irradiates the sample in the nuclear magnetic tube.

[0017] In some embodiments, the fiber optic component in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe includes a fiber optic and a front-end coupler and a rear-end coupler respectively connected to the front end and the rear end of the fiber optic. The front end of the fiber optic is connected to the laser, and the other end passes through the bottom of the nuclear magnetic resonance probe, passes through the newly designed bypass inside the probe, and is connected to the ferrule component.

[0018] In some embodiments, the fiber optic in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe has an insulating cladding at its front end, no insulating cladding at its rear end, and the diameter of the rear end of the fiber optic is less than 2 mm.

[0019] In some embodiments, the optical mirror component in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe includes a lens and a corner mirror. In the direction of laser emission, the corner mirror is located in front of the lens, and both the lens and the corner mirror are arranged on the ferrule component.

[0020] In some embodiments, the ferrule assembly in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe includes a ferrule, and the lens and the corner reflector are respectively installed in the ferrule in the laser emission direction.

[0021] In some embodiments, the ferrule in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe is made of a non-magnetic material and has a metal layer on its inner wall.

[0022] In some embodiments, one end of the ferrule in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe is a stepped circular ring structure matching the structure of the nuclear magnetic resonance probe base. The ferrule assembly further includes a ferrule cover provided at the other end of the ferrule. The ferrule cover is provided with a through hole for inserting and fixing a nuclear magnetic resonance tube containing a sample, and the sample is surrounded by a radio frequency coil.

[0023] In some embodiments, one end of the ferrule in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe matches the structure of the upper half of the nuclear magnetic resonance probe base and can rotate relative to the nuclear magnetic resonance probe base. The lens is embedded at one end of the ferrule, and the corner reflector is also fixed on the ferrule, in front of the lens. The spot size thereof can be adjusted by the lens, and the reflection light direction can be adjusted with the rotation of the ferrule, so as to maximize the transmission of the light source through the radio frequency coil to irradiate the sample in the nuclear magnetic resonance tube.

[0024] In some embodiments, through the fiber collimating reflective rotatable optical path transmission system in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe, a sufficient and uniform light source can be provided for the sample.

[0025] In some embodiments, a protective sleeve is sleeved outside the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe.

[0026] In some embodiments, the laser is a high-power continuous laser.

[0027] In some embodiments, the in-situ photocatalytic nuclear magnetic resonance detection device can provide a full-band light source including ultraviolet light, visible light, and infrared light by configuring different lasers.

[0028] In some embodiments, the in-situ photocatalytic nuclear magnetic resonance detection device can conduct research on the photocatalytic reaction mechanism and kinetics under in-situ conditions through a data acquisition system for real-time monitoring and a nuclear magnetic resonance variable temperature system.

[0029] In addition, although the ferrule assembly, the optical fiber assembly, and the optical mirror assembly are optimized according to the internal structure and spatial size of the probe we designed, for probes with a simple internal structure and a large space, we can also optimize the dimensions, shapes, etc. of the ferrule assembly, the optical fiber assembly, and the optical mirror assembly according to actual needs to make them suitable for different types of probes.

[0030] Moreover, since the ferrule assembly we designed is non-magnetic, we can also adjust the structure size of the optical path assembly we designed according to actual needs and place it in any reaction device or detection device with a strong magnetic field to achieve photocatalytic reactions or in-situ photocatalytic detection.

[0031] Therefore, in some embodiments, the probe can be replaced with a reaction device or a detection device with a strong magnetic field, and the dimensions, shapes, etc. of the optical path assembly can be adjusted according to the structure of the reaction device or the detection device. Specifically, the detection device can also be a probe with a simple internal structure and a large space.

[0032] Based on the disclosure of the above embodiments, the beneficial effects of the embodiments of the present invention include:

[0033] (1) The present invention designs a "collimated reflection type" light source input system for the nuclear magnetic resonance probe, non-invasively modifies the nuclear magnetic resonance probe, and can provide a uniform light source with full wavelength bands and high intensity, enabling it to have the ability to perform in-situ photocatalytic reactions and detect the nuclear magnetic resonance signals of photocatalytic products at the same time.

[0034] (2) The optical fiber assembly designed by the present invention has adjustability and can easily switch different irradiation wavelengths. In this way, we can select the most suitable wavelength for photocatalytic experiments or in-situ photocatalytic detection according to needs and ensure uniform light intensity.

[0035] (3) The ferrule assembly designed by the present invention is used to support and limit the optical fiber assembly and the optical mirror assembly, and can stably place the optical fiber assembly and the optical mirror assembly inside the probe. This ensures the tight combination of the optical components and the probe, enabling them to be stably placed inside the probe.

[0036] (4) The optical mirror assembly designed by the present invention is placed inside the nuclear magnetic resonance probe. In order to achieve the effect of high-power uniform illumination of the sample, the focal length of the lens and the distance between the lens and the mirror are designed according to the size of the nuclear magnetic resonance sample tube to control the size of the light spot, which is used to converge, collimate, and adjust the direction and size of the laser beam emitted by the optical fiber assembly.

[0037] (5) By designing and using a high-quality light source system, optical fiber components, ferrule components, and optical mirror components, the present invention can maximize the sensitivity and accuracy of in-situ photocatalytic nuclear magnetic detection. Combining with a data acquisition system for real-time monitoring and a nuclear magnetic variable temperature system, it provides a new technical means for studying the photocatalytic reaction mechanism and kinetics under in-situ conditions. Moreover, the components are convenient to disassemble, reserving space for introducing new functions into the probe in the future.

[0038] Other features and advantages of the present invention will be described in the following specification. And, in part, they will become obvious from the specification or be understood by implementing the present invention. The objectives and other advantages of the present invention can be achieved and obtained through the structure specifically pointed out in the written specification and the accompanying drawings.

[0039] The technical solutions of the present invention will be further described in detail below through the accompanying drawings and embodiments. Description of the Drawings

[0040] To more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments recorded in the present application. At the appropriate time, the same reference numerals will be used to refer to the same or similar parts in all the drawings. Such embodiments are illustrative and are not intended to be an exhaustive or exclusive embodiment of the present device or method. In the drawings:

[0041] Figure 1 It is a schematic structural diagram of a fiber optic collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe in an embodiment of the present invention.

[0042] Figure 2 It is a schematic structural diagram of a fiber optic collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe in an embodiment of the present invention.

[0043] Figure 3 It is a partial schematic structural diagram of a fiber optic collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe in an embodiment of the present invention.

[0044] Figure 4 It is a partial schematic structural diagram of a fiber optic collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe in an embodiment of the present invention.

[0045] Figure 5 It is a partial schematic structural diagram of an optical fiber in an embodiment of the present invention.

[0046] Reference Numerals:

[0047] 1 - Nuclear magnetic resonance probe; 2 - Laser; 3 - Optical fiber components; 4 - Optical mirror components; 5 - Ferrule components; 6 - Optical fiber Detailed Embodiments

[0048] Next, specific embodiments of the present invention will be described in detail with reference to the accompanying drawings, but this is not intended to limit the present invention.

[0049] It should be understood that various modifications can be made to the embodiments disclosed herein. Therefore, the following description should not be regarded as restrictive, but only as an example of the embodiments. Those skilled in the art will think of other modifications within the scope and spirit of the present disclosure.

[0050] The accompanying drawings included in the specification and forming a part of the specification illustrate embodiments of the present disclosure, and together with the general description of the present disclosure given above and the detailed description of the embodiments given below are used to explain the principles of the present disclosure.

[0051] These and other features of the present invention will become apparent from the following description of the preferred forms of the embodiments given as non - limiting examples with reference to the accompanying drawings.

[0052] It should also be understood that although the present invention has been described with reference to some specific examples, those skilled in the art can surely implement many other equivalent forms of the present invention, which have the features as described above and thus are all within the protection scope defined thereby.

[0053] When combined with the accompanying drawings, the above - mentioned and other aspects, features, and advantages of the present disclosure will become more apparent in view of the following detailed description.

[0054] Hereinafter, specific embodiments of the present disclosure will be described with reference to the accompanying drawings; however, it should be understood that the disclosed embodiments are merely examples of the present disclosure, which can be implemented in various ways. Well - known and / or repetitive functions and structures are not described in detail to avoid obscuring the present disclosure with unnecessary or redundant details. Therefore, the specific structural and functional details disclosed herein are not intended to be limiting, but merely as a basis and representative basis for teaching those skilled in the art to use the present disclosure in substantially any suitable detailed structure in a variety of ways.

[0055] This specification may use the phrase "in one embodiment", "in another embodiment", "in yet another embodiment", or "in other embodiments", which may each refer to one or more of the same or different embodiments according to the present disclosure.

[0056] Next, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

[0057] As Figure 1 、 Figure 2 、 Figure 3 and Figure 4 shown, an in - situ photocatalytic nuclear magnetic detection device provided by an embodiment of the present invention includes:

[0058] Fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe 1, which is used for in-situ photocatalytic reaction and the reception of nuclear magnetic resonance signals during the reaction process. The optical fiber component 3 in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe 1 is connected to an external laser 2 and extends into the nuclear magnetic resonance probe 1 to introduce laser light into the nuclear magnetic resonance probe 1. The optical mirror component 4 in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe 1 is arranged inside the nuclear magnetic resonance probe 1 and is used for converging, collimating and adjusting the direction of the laser light emitted by the optical fiber component 3. The ferrule component 5 in the fiber collimating reflective full-band in-situ photocatalytic nuclear magnetic resonance probe 1 is arranged inside the nuclear magnetic resonance probe 1 and is used for supporting and limiting the optical fiber component and the optical mirror component;

[0059] Laser 2, which is used to provide the light source required for the photocatalytic reaction;

[0060] Magnet, cabinet and nuclear magnetic resonance signal real-time acquisition system: matching with the nuclear magnetic resonance probe to obtain the nuclear magnetic resonance signals of the photocatalytic reaction system.

[0061] Based on the disclosure of the above embodiments, it can be known that the beneficial effects of this embodiment include that the in-situ photocatalytic nuclear magnetic resonance probe can provide effective light energy for the in-situ photocatalytic reaction and can collect the nuclear magnetic resonance signals during the photocatalytic process of the system in real time, thereby providing a new technical means for the research of photocatalytic reaction mechanism and kinetics. Moreover, the relevant components in the probe are convenient to disassemble, leaving room for introducing new functions into the probe in the future. The in-situ photocatalytic nuclear magnetic resonance probe of this embodiment is used to collect nuclear magnetic resonance signals in real time during the photocatalytic reaction process. The probe of this embodiment combines the optical path building technology and nuclear magnetic resonance technology. The optical path building technology is responsible for introducing laser light with appropriate power and size into the nuclear magnetic tube to initiate the photocatalytic reaction; the nuclear magnetic resonance technology is responsible for monitoring the chemical composition changes during the photocatalytic reaction process under the action of the superconducting magnetic field in real time.

[0062] Specifically, the laser 2 of this embodiment is a high-power continuous laser 2, which includes a laser power supply and a laser head, and has excellent optical stability, and the optical stability value is less than 5%. The emission wavelength of the laser 2 can be 450 nanometers. Of course, lasers 2 with other wavelengths can also be used for replacement to cover the spectral ranges of ultraviolet light, visible light and near-infrared regions. Moreover, the power of the laser 2 is adjustable. The maximum power of the laser 2 with an emission wavelength of 450 nanometers selected in this embodiment is 4 watts.

[0063] Further, the optical fiber component 3 includes an optical fiber 6 and a front-end coupler and a rear-end coupler respectively connected to the front end and the rear end of the optical fiber 6. The front end of the optical fiber 6 is connected to the laser 2, and the rear end is connected to the ferrule component 5.

[0064] Specifically, the front end of the optical fiber 6 has an insulating cladding, the rear end of the optical fiber 6 has no insulating cladding, and the diameter of the rear end of the optical fiber 6 is less than 2 mm.

[0065] Exemplarily, as Figure 5 shown, the front end portion of the optical fiber 6 is composed of a bare optical fiber and a cladding, and is equipped with a front end coupler. For example, it can be connected to the laser 2 through the SMA90 connector port to ensure stable output of the laser. Since the optical fiber 6 needs to pass through the entire in-situ photocatalytic NMR probe 1, its diameter must be less than 2 mm. Based on this, in this embodiment, the rear end portion of the optical fiber is a bare optical fiber without a cladding, so as to facilitate controlling the size of the rear end of the optical fiber and enabling it to extend into the in-situ photocatalytic NMR probe 1.

[0066] Furthermore, the light-emitting end of the optical fiber 6 in this embodiment is configured with a light-emitting port, and the ferrule assembly 5 is arranged in front of it. The light-emitting port of the optical fiber 6 is made of a customized non-magnetic material, such as plastic, copper, aluminum, non-magnetic tungsten steel, etc., to ensure compatibility with the NMR instrument. During application, the length of the optical fiber exceeds 3 meters, and the part connected to the laser 2 can be 2 meters. This part is provided with a protective sleeve, that is, a cladding, while the part connected to the NMR probe is a bare optical fiber. One end of the optical fiber 6 enters the interior of the NMR instrument and is fixed through a customized non-magnetic ferrule, that is, the light-emitting port.

[0067] In addition, since the optical fiber 6 in the NMR probe is a bare optical fiber, the path through which it passes through the probe needs to be precisely arranged according to the structure of the probe, and the port processing is carried out after passing through each part of the probe. Because the diameter of the port will be greater than 2 mm, if the optical fiber port is installed in advance, the penetration of the optical fiber through each part of the NMR probe cannot be achieved.

[0068] Furthermore, the optical mirror assembly 4 includes a lens and a corner reflector. In the laser emission direction, the corner reflector is located in front of the lens, and both the lens and the corner reflector are arranged on the ferrule assembly 5.

[0069] Furthermore, the ferrule assembly 5 includes a ferrule, and the lens and the corner reflector are respectively installed in the ferrule in the laser emission direction. For example, a small lens is embedded at the bottom of the ferrule to prevent the light transmitted by the optical fiber from diverging. A 45-degree corner reflector is embedded in the ferrule in front of the lens to adjust the light source direction so that it irradiates the NMR sample.

[0070] The ferrule in this embodiment is made of non-magnetic material. A metal layer is provided on the inner wall, and the specific metal is not limited. One end of the ferrule is structurally matched with the in-situ photocatalytic NMR probe 1 and can rotate relative to the in-situ photocatalytic NMR probe 1. For example, the structure of one end of the ferrule and the in-situ photocatalytic NMR probe 1 is a matching stepped circular ring structure. The lens is embedded at one end of the ferrule, and the angular reflector is embedded in front of the lens. In addition, the ferrule assembly 5 further includes a ferrule cover provided at the other end of the ferrule. The ferrule cover can also be fixed to the ferrule through a stepped circular ring structure and can rotate relative to the ferrule. The ferrule cover is provided with a through hole for inserting and fixing an NMR tube containing a sample, and the sample is surrounded by a radio frequency coil.

[0071] Exemplarily, the ferrule in this embodiment is a non-magnetic precision-machined ferrule for fixing optical elements and positioning the NMR tube, and its dimensions are precisely matched with the components of the NMR probe base. The ferrule material is non-magnetic material, such as alumina or polytetrafluoroethylene, etc. The bottom of the ferrule is matched with the stepped circular ring structure of the NMR probe and can be moderately rotated to adjust the optimal light intensity of the incident light. The inner layer of the ferrule can be treated with gold plating or silver plating to increase the probability of light irradiation, reduce light loss, and improve photocatalytic activity. The top of the ferrule is matched with the ferrule cover through a stepped circular ring structure. The center of the ferrule cover is provided with a round hole for inserting and fixing an NMR tube containing a sample, and the sample part is surrounded by a radio frequency coil.

[0072] Furthermore, the non-magnetic precision-machined ferrule also needs to leave appropriate positions and dimensions to embed a small lens and a small angular reflector. The small lens is used to modulate the laser spot size and collimate. The small angular reflector is fixed at 45 degrees with the collimation direction of the small lens to cooperate to turn the laser emitted from back to front to the horizontal direction, and then irradiate the inside of the NMR sample through the transparent radio frequency coil. The NMR tube is inserted into the ferrule cover, and the internal sample is surrounded by a radio frequency coil.

[0073] Furthermore, since the RF coils in the NMR tube are densely arranged, the laser is likely to hit the surroundings of the RF coils and be reflected, preventing the laser from the laser source from hitting the sample. Moreover, if the laser spot is too small, only a very small area of the sample will be irradiated by the high power of the laser, and the excited area is extremely uneven, which easily leads to burning out the sample. To solve the above two problems, the diameter of the laser spot hitting the sample in this embodiment is designed to be 15 mm, so as to ensure that most areas in the sample tube are evenly irradiated by light. At the same time, the metal reflective film on the inner wall of the collar can also reflect the light hitting the RF coils multiple times, increasing the probability of the light source hitting the sample and facilitating the photocatalytic reaction. To ensure that the laser spot size is 15 mm, it is necessary to accurately design the distance between the corner reflector and the sample and the distance between the lens and the corner reflector according to the emission angle of the optical fiber. Specifically, the thickness, diameter and positioning of the optical components can be theoretically calculated through geometric optics theory, and the corresponding optical components can be made using customized molds, and then modularly and accurately assembled.

[0074] As another alternative embodiment, to ensure structural stability, in this embodiment, a protective sleeve is sleeved outside the NMR probe. For example, it is a non-magnetic metal long cylinder, which is used to lock the probe, the collar and all other components to prevent the components from being unstable or falling off during the test.

[0075] In this embodiment, through the in-situ photocatalytic NMR detection device, real-time NMR signal monitoring and detection during the photocatalytic process of liquid samples are realized, ensuring the consistency of the chemical reaction environment control. Moreover, by selecting non-magnetic materials, the interference of magnetism on the NMR cavity and NMR signals can be effectively avoided. In addition, the in-situ photocatalytic NMR detection device can directly fix the optical fiber, lens and corner reflector on the base of the probe using a customized collar, which is easy to operate.

[0076] The above description is only the preferred solution of this embodiment and the description of the technical principles applied. Those skilled in the art should understand that the protection scope of the present disclosure is not limited to the combination of the above specific technical features, but should also include other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the concept of the present disclosure. For example, the technical solutions formed by mutually replacing the above features with technical features having similar functions in the present disclosure.

[0077] In addition, although the operation steps are described in a specific order, it should not be understood as requiring execution in the order shown. In some cases, multitasking and parallel processing may be beneficial. Similarly, although several specific implementation details are included in the discussion, these should not be construed as limitations on the scope of the present disclosure. Some features described in separate embodiments can be combined and implemented, and vice versa.

[0078] Although the subject matter has been described in language specific to structural features and / or methodological logical acts, it is to be understood that the claimed subject matter is not limited to the specific features or acts described above. The specific features and acts described above are only example forms of implementation.

[0079] The above has described in detail multiple embodiments of the present disclosure, but the present disclosure is not limited to these specific embodiments. Based on the concept of the present disclosure, those skilled in the art can make various variations and modifications to the embodiments, and these variations and modifications should all be included within the scope claimed by the present disclosure.

Claims

1. An in-situ photocatalytic nuclear magnetic detection device, characterized in that, Comprising: An optical fiber collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe, which is used for in-situ photocatalytic reaction and receiving the nuclear magnetic resonance signals of compounds during the reaction process. The optical fiber component in the optical fiber collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe is connected to an external laser and extends into the nuclear magnetic resonance probe to introduce the laser into the nuclear magnetic resonance probe. The optical mirror component in the optical fiber collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for converging, collimating and adjusting the direction of the laser emitted by the optical fiber component. The ferrule component in the optical fiber collimating and reflecting full-band in-situ photocatalytic nuclear magnetic resonance probe is arranged inside the nuclear magnetic resonance probe and is used for supporting and limiting the optical fiber component and the optical mirror component. The ferrule component includes a ferrule; the laser is used to provide the light source required for the photocatalytic reaction. A magnet, a cabinet and a nuclear magnetic resonance signal real-time acquisition system, which are matched with the nuclear magnetic resonance probe to obtain the nuclear magnetic resonance signals of the compounds in the reaction system during the photocatalytic process and monitor the progress of the photocatalytic reaction. The optical path design inside the nuclear magnetic resonance probe adopts a collimating and reflecting scheme, including designing an optical path independent of the key probe components such as the tuning bar, the temperature control device, the capacitor, and the transmit / receive coil at the edge position inside the nuclear magnetic resonance probe and capable of accommodating a 2-mm optical fiber. One end of the optical fiber is connected to the laser, and the other end passes through the bottom of the nuclear magnetic resonance probe and is connected to the ferrule component that matches the main structure of the nuclear magnetic resonance probe through a newly designed bypass inside the nuclear magnetic resonance probe. The light source input into the probe is reflected by the angular mirror embedded in the ferrule component, passes through the gap of the radio frequency coil, and irradiates the sample in the nuclear magnetic tube. The optical mirror component includes a lens and an angular mirror. In the direction of the laser emission, the angular mirror is located in front of the lens. Both the lens and the angular reflecting mirror are arranged inside the ferrule of the ferrule component. One end of the ferrule is matched with the structure of the upper half base of the nuclear magnetic resonance probe and can rotate relative to the base of the nuclear magnetic resonance probe. The lens is embedded at one end of the ferrule, and the angular mirror is also fixed on the ferrule and is located in front of the lens. The size of its light spot can be adjusted by the lens, and the direction of the reflected light can be adjusted with the rotation of the ferrule to maximize the light source passing through the radio frequency coil and irradiating the sample in the nuclear magnetic tube.

2. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, characterized in that, The optical fiber component includes an optical fiber and a front-end coupler and a rear-end coupler respectively connected to the front end and the rear end of the optical fiber. The front end of the optical fiber is connected to the laser, and the other end passes through the bottom of the nuclear magnetic resonance probe and is connected to the ferrule component in the probe through a newly designed bypass inside the probe.

3. The in-situ photocatalytic nuclear magnetic detection device according to claim 2, characterized in that The front end of the optical fiber has an insulating cladding, the rear end of the optical fiber has no insulating cladding, and the diameter of the rear end of the optical fiber is less than 2 mm.

4. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, characterized in that, The ferrule is made of a non-magnetic material, and a metal layer is provided on the inner wall.

5. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, wherein One end of the ferrule is a stepped circular ring structure that matches the structure of the base of the nuclear magnetic resonance probe. The ferrule component further includes a ferrule cover arranged at the other end of the ferrule. The ferrule cover is provided with a through hole for inserting and fixing the nuclear magnetic tube containing the sample, and the sample is surrounded by the radio frequency coil.

6. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, characterized in that A protective sleeve is sleeved outside the nuclear magnetic resonance probe.

7. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, wherein the laser is a high-power continuous laser.

8. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, characterized in that By configuring different lasers, a full-spectrum light source including ultraviolet light, visible light, and infrared light is provided.

9. The in-situ photocatalytic nuclear magnetic detection device according to claim 1, characterized in that Through real-time monitoring by the data acquisition system and the nuclear magnetic variable temperature system, the photocatalytic reaction mechanism and kinetics can be studied under in-situ conditions.

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