In-situ quantitative sampling device of hydrothermal high-pressure reaction kettle

Abstract

The utility model discloses an in-situ quantitative sampling device of a hydrothermal high-pressure reaction kettle, which comprises a heat exchange assembly and a fluid pipeline assembly, the heat exchange assembly is provided with a sampling cavity and a heat exchange cavity, heat in the sampling cavity can be transferred to the heat exchange cavity, and the fluid pipeline assembly is provided with a first stop valve and a second stop valve. The inlet end of the first stop valve is communicated with the outlet end of the hydrothermal high-pressure reaction kettle, the outlet end of the first stop valve is communicated with the inlet end of the sampling cavity, and the inlet end of the second stop valve is communicated with the outlet end of the sampling cavity. The in-situ quantitative sampling can be carried out on the hydrothermal high-pressure reaction kettle in operation, the operation is very simple and convenient, and the sampling is more accurate.

Description

Technical Field

[0001] The utility model relates to the technical field of biochemical reaction sampling, in particular to an in-situ quantitative sampling device for a hydrothermal high-pressure reactor. Background Art

[0002] In the related art, hydrothermal technology, as an environmentally friendly technology, is widely used in the synthesis and preparation of materials in the field of materials science, the treatment of solid waste in the field of environmental science, and the production of products in the field of chemical industry. The principle of hydrothermal technology is to use aqueous solution as the reaction medium in a special closed reaction container (such as a hydrothermal autoclave), and to create a high-temperature and high-pressure reaction environment by heating the container, so that the insoluble or insoluble substances undergo processes such as dissolution and recrystallization. A hydrothermal autoclave is a closed high-temperature and high-pressure container that uses hydrothermal reaction to promote the decomposition and transformation of substances. Sampling during the hydrothermal reaction process can explore the material transformation and product synthesis at different stages. However, due to the danger of high-temperature and high-pressure sampling, the existing sampling method is to open the sampling after the reaction is completed and the reactor is cooled to room temperature. The existing high-pressure reactor sampling device cannot meet the requirements of in-situ sampling, which makes it very difficult for experimenters to study the transformation path and chemical kinetics of the substance, which is not conducive to the development and optimization of products; in addition, sampling will be affected by the sampling tools and sampling personnel, and improper operation during the sampling process will lead to the accuracy and precision of the experimental data cannot be guaranteed. Utility Model Content

[0003] The utility model aims to solve at least one of the technical problems existing in the prior art. To this end, the utility model provides an in-situ quantitative sampling device for a hydrothermal high-pressure reactor, which can realize in-situ sampling.

[0004] The in-situ quantitative sampling device of the hydrothermal high-pressure reactor of the utility model embodiment comprises:

[0005] A heat exchange component, wherein the heat exchange component has a sampling cavity and a heat exchange cavity, and the heat in the sampling cavity can be transferred to the heat exchange cavity;

[0006] A fluid pipeline assembly, wherein the fluid pipeline assembly is provided with a first stop valve and a second stop valve, wherein the inlet end of the first stop valve is connected to the outlet end of the hydrothermal high-pressure reactor, the outlet end of the first stop valve is connected to the inlet end of the sampling chamber, and the inlet end of the second stop valve is connected to the outlet end of the sampling chamber.

[0007] The in-situ quantitative sampling device for the hydrothermal high-pressure reactor of the embodiment of the utility model can perform in-situ quantitative sampling of the hydrothermal high-pressure reactor in operation by operating the first stop valve and the second stop valve according to the needs of the experimenter. The operation is very simple and the sampling is more accurate.

[0008] According to some embodiments of the utility model, the heat exchange assembly is provided with a first cylinder and a second cylinder, the second cylinder is arranged on the outside of the first cylinder, the inner cavity of the first cylinder constitutes the sampling cavity, and the cavity formed by the second cylinder and the first cylinder constitutes the heat exchange cavity.

[0009] According to some embodiments of the present utility model, the second cylinder is connected to a first cooling tube and a second cooling tube, the first cooling tube is used to input cooling liquid into the heat exchange cavity, and the second cooling tube is used to discharge the cooling liquid in the heat exchange cavity.

[0010] According to some embodiments of the present invention, the first cooling pipe is connected to the outer side wall of the lower end of the second cylinder, and the second cooling pipe is connected to the outer side wall of the upper end of the second cylinder.

[0011] According to some embodiments of the present invention, an anti-slip structure is provided at the end of the first cooling tube and / or the second cooling tube away from the second cylinder.

[0012] According to some embodiments of the utility model, the sampling device also includes a pressure gauge, and the fluid pipeline assembly is also provided with a first three-way joint, a second three-way joint and a third stop valve, the outlet end of the first stop valve is connected to the inlet end of the first three-way joint through a first fluid pipe, one of the outlet ends of the first three-way joint is connected to the inlet end of the second three-way joint through a second fluid pipe, the other outlet end of the first three-way joint is connected to the sampling chamber through a third fluid pipe, the pressure gauge is connected to one of the outlet ends of the second three-way joint, and the inlet end of the third stop valve is connected to the other outlet end of the second three-way joint through a fourth fluid pipe.

[0013] According to some embodiments of the present utility model, the first three-way joint and the second three-way joint are both ferrule-type three-way joints, and the first stop valve, the second stop valve and the third stop valve are all ferrule-type stop valves.

[0014] According to some embodiments of the present invention, the heat exchange assembly further includes a first ferrule joint, one end of which is connected to the upper end of the first cylinder, and the other end of which is sleeved on the outer wall of the third fluid pipe.

[0015] According to some embodiments of the present invention, one end of the third fluid tube away from the first three-way connector extends into the sampling cavity, and an outlet end of the third fluid tube is close to an outlet end of the sampling cavity.

[0016] According to some embodiments of the present invention, the heat exchange assembly further comprises a second ferrule joint, one end of which is connected to the lower end of the first cylinder, and the other end of which is connected to the inlet end of the second stop valve through a fifth fluid pipe.

[0017] Additional aspects and advantages of the present invention will be given in part in the following description, and in part will become apparent from the following description, or will be learned through the practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The present invention is further described below with reference to the accompanying drawings and embodiments, wherein:

[0019] Figure 1 This is a schematic structural diagram of an in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to an embodiment of the utility model (used for sampling liquid samples);

[0020] Figure 2 This is a schematic structural diagram of an in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to an embodiment of the utility model (used for sampling gas phase samples and liquid phase samples);

[0021] Reference numerals:

[0022] 1. Pressure gauge; 2. Heat exchange assembly; 21. Sampling chamber; 22. Heat exchange chamber; 23. First cooling tube; 231. First protruding structure; 24. Second cooling tube; 241. Second protruding structure; 311. First stop valve; 312. Second stop valve; 313. Third stop valve; 321. First three-way joint; 322. Second three-way joint; 331. First fluid pipe; 332. Second fluid pipe; 333. Third fluid pipe; 334. Fourth fluid pipe; 335. Fifth fluid pipe; 341. First ferrule joint; 342. Second ferrule joint; DETAILED DESCRIPTION

[0023] The embodiments of the present invention are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0024] In the description of the present invention, it should be understood that descriptions involving orientation, such as up, down, front, back, left, right, etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0025] In the description of the present utility model, "several" means one or more, "more" means more than two, "greater than", "less than", "exceed" etc. are understood to exclude the number itself, and "above", "below", "within" etc. are understood to include the number itself. If there is a description of "first" or "second", it is only used for the purpose of distinguishing the technical features, and cannot be understood as indicating or implying the relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0026] In the description of the present invention, unless otherwise clearly defined, terms such as setting, installing, connecting, etc. should be understood in a broad sense, and technicians in the relevant technical field can reasonably determine the specific meanings of the above terms in the present invention based on the specific content of the technical solution.

[0027] In the related art, hydrothermal technology, as an environmentally friendly technology, is widely used in the synthesis and preparation of materials in the field of materials science, the treatment of solid waste in the field of environmental science, and the production of products in the field of chemical industry. The principle of hydrothermal technology is to use aqueous solution as the reaction medium in a special closed reaction container (such as a hydrothermal autoclave), and to create a high-temperature and high-pressure reaction environment by heating the container, so that the insoluble or insoluble substances undergo processes such as dissolution and recrystallization. A hydrothermal autoclave is a closed high-temperature and high-pressure container that uses hydrothermal reaction to promote the decomposition and transformation of substances. Sampling during the hydrothermal reaction process can explore the material transformation and product synthesis at different stages. However, due to the danger of high-temperature and high-pressure sampling, the existing sampling method is to open the sampling after the reaction is completed and the reactor is cooled to room temperature. The existing high-pressure reactor sampling device cannot meet the requirements of in-situ sampling, which makes it very difficult for experimenters to study the transformation path and chemical kinetics of the substance, which is not conducive to the development and optimization of products; in addition, sampling will be affected by the sampling tools and sampling personnel, and improper operation during the sampling process will lead to the accuracy and precision of the experimental data cannot be guaranteed.

[0028] To this end, the utility model provides an in-situ quantitative sampling device for a hydrothermal high-pressure reactor, which can realize in-situ sampling and improve the accuracy of sampling data.

[0029] Reference Figure 1 to Figure 2In some embodiments of the present invention, a hydrothermal autoclave in-situ quantitative sampling device includes a heat exchange component 2 and a fluid pipeline component. The heat exchange component 2 has a sampling chamber 21 and a heat exchange chamber 22. The heat in the sampling chamber 21 can be transferred to the heat exchange chamber 22. The fluid pipeline component is provided with a first stop valve 311 and a second stop valve 312. The inlet end of the first stop valve 311 is connected to the outlet end of the hydrothermal autoclave, and the outlet end of the first stop valve 311 is connected to the inlet end of the sampling chamber 21. Therefore, by opening the first stop valve 311, the sample in the hydrothermal autoclave can be quantitatively entered into the sampling chamber 21. The inlet end of the second stop valve 312 is connected to the outlet end of the sampling chamber 21. Therefore, after the sample is cooled down in the sampling chamber 21 through heat exchange, the cooled sample can be discharged for collection and analysis by opening the second stop valve 312. Specifically, the heat exchange chamber 22 can be arranged at the periphery of the sampling chamber 21. For example, the heat exchange chamber 22 is arranged in a spiral tube shape around the outside of the sampling chamber 21, so that the heat exchange area between the two is larger, which is conducive to improving the efficiency of heat exchange. Of course, the sampling chamber 21 can also be arranged at the periphery of the heat exchange chamber 22. When sampling, cooling water or cooling oil or other types of coolants are introduced into the heat exchange chamber 22. At this time, the heat of the sample in the sampling chamber 21 can be transferred to the coolant in the heat exchange chamber 22, so that the temperature of the sample can be quickly reduced. Finally, the sample is discharged through the second stop valve 312 to be collected for specific analysis.

[0030] The in-situ quantitative sampling device for the hydrothermal high-pressure reactor of the embodiment of the utility model can perform in-situ quantitative sampling of the hydrothermal high-pressure reactor in operation by operating the first stop valve 311 and the second stop valve 312 according to the needs of the experimenter. The operation is very simple and the sampling is more accurate.

[0031] It is understandable that in order to achieve rapid cooling of the sample, in some embodiments of the present utility model, the heat exchange component 2 is provided with a first cylinder and a second cylinder, the second cylinder is arranged on the outside of the first cylinder, the inner cavity of the first cylinder constitutes a sampling cavity 21, and the cavity formed by the second cylinder and the first cylinder constitutes a heat exchange cavity 22. When the cooling liquid is input into the second cylinder, the cooling liquid can be well coated on the outer wall of the sampling cavity 21. At this time, the heat of the sample in the sampling cavity 21 can be transferred to the cooling liquid through the outer wall of the sampling cavity 21, so that the temperature of the sample can be quickly reduced. Specifically, according to the quantitative sampling requirements, first cylinders with different outer diameters can be designed to obtain sampling cavities 21 of different volumes, and then the corresponding second cylinders can be matched to meet the different quantitative sampling requirements of different samples.

[0032] It can be understood that in order to further improve the speed of sample cooling, in some embodiments of the present invention, the second cylinder is connected to the first cooling tube 23 and the second cooling tube 24, the first cooling tube 23 is used to input cooling liquid into the heat exchange chamber 22, and the second cooling tube 24 is used to discharge the cooling liquid in the heat exchange chamber 22. Of course, a cooling pump and a cooling pool can also be provided on the outside. The cooling pump circulates the cooling liquid between the first cooling tube 23, the heat exchange chamber 22, the second cooling tube 24 and the cooling pool, so that the cooling liquid in the heat exchange chamber 22 can circulate and quickly dissipate the heat to the outside, so that the cooling liquid can accelerate the absorption of the heat of the sample and improve the speed of sample cooling.

[0033] It is understandable that, in order to further improve the heat exchange efficiency of the coolant, in some embodiments of the present invention, the first cooling tube 23 is connected to the outer wall of the lower end of the second cylinder, and the second cooling tube 24 is connected to the outer wall of the upper end of the second cylinder. Since the sample is discharged from the sampling cavity 21 from the lower end of the first cylinder, by connecting the first cooling tube 23 to the outer wall of the lower end of the second cylinder, the coolant first contacts the outer wall of the lower end of the first cylinder when passing from the first cooling tube 23 into the heat exchange cavity 22, so that the sample to be discharged from the sampling cavity 21 can be further cooled, thereby further improving the heat exchange efficiency of the coolant, so that the temperature of the sample can be reduced to a lower level.

[0034] It is understandable that the first cooling pipe 23 and the second cooling pipe 24 usually need to be connected to a delivery hose to deliver the coolant to a cooling pump, a cooling pool or other external equipment. However, during the circulation of the coolant, the delivery hose will vibrate and may cause the delivery hose to fall off from the first cooling pipe 23 and / or the second cooling pipe 24. For this reason, in some embodiments of the utility model, the first cooling pipe 23 and / or the second cooling pipe 24 are provided with a stop structure at the end away from the second cylinder. The stop structure can increase the connection force between the delivery hose and the first cooling pipe 23 and the second cooling pipe 24, thereby effectively preventing the delivery hose from falling off from the first cooling pipe 23 and the second cooling pipe 24, improving the stability of the device operation, and thus improving the reliability of sampling. Specifically, the stop structure can be a plurality of protrusions with a certain taper, or a threaded structure, or other structures, which can be specifically set according to actual needs. For example, the anti-slip structure of the first cooling tube 23 is a first protruding structure 231 with a certain taper, and the anti-slip structure of the second cooling tube 24 is a second protruding structure 241 with a certain taper. The first protruding structure 231 and the second protruding structure 241 can be the same structure or different structures.

[0035] It can be understood that in order to monitor and collect the gas phase sample in the sample in real time, in some embodiments of the present utility model, the sampling device also includes a pressure gauge 1, and the fluid pipeline assembly is also provided with a first three-way joint 321, a second three-way joint 322 and a third stop valve 313, the outlet end of the first stop valve 311 is connected to the inlet end of the first three-way joint 321 through the first fluid pipe 331, one of the outlet ends of the first three-way joint 321 is connected to the inlet end of the second three-way joint 322 through the second fluid pipe 332, the other outlet end of the first three-way joint 321 is connected to the sampling chamber 21 through the third fluid pipe 333, the pressure gauge 1 is connected to one of the outlet ends of the second three-way joint 322, and the inlet end of the third stop valve 313 is connected to the other outlet end of the second three-way joint 322 through the fourth fluid pipe 334. When the sample enters the inlet end of the first stop valve 311 from the outlet end of the hydrothermal high-pressure reactor, the gas phase of the sample will pass through the first fluid pipe 331, the first three-way joint 321, the second fluid pipe 332, the second three-way joint 322, the fourth fluid pipe 334, and the third stop valve 313 in sequence, wherein the pressure gauge 1 is connected to an outlet end of the second three-way joint 322, so the pressure gauge 1 can monitor the sampling pressure value in real time. When the non-condensable gas in the sample needs to be collected after the sample is cooled, the third stop valve 313 can be opened so that the non-condensable gas can be discharged through the outlet end of the third stop valve 313, thereby facilitating the experimenter to collect and analyze the gas phase sample. In addition, at this time, the liquid phase in the sample is discharged through the outlet end of the second stop valve 312, thereby facilitating the experimenter to collect and analyze the liquid phase sample.

[0036] It is understandable that, in order to facilitate installation and disassembly of the device, in some embodiments of the present invention, the first three-way connector 321 and the second three-way connector 322 are both ferrule-type three-way connectors, and the first stop valve 311, the second stop valve 312 and the third stop valve 313 are all ferrule-type stop valves, so that the device is very convenient to operate during installation and disassembly, and only the corresponding ferrules need to be twisted. Of course, since the device adopts the above structure, the cleaning, maintenance and component replacement of the device are very convenient.

[0037] It can be understood that in order to facilitate the fixation of the third fluid tube 333, in some embodiments of the present invention, the heat exchange assembly 2 also includes a first ferrule joint 341, one end of the first ferrule joint 341 is connected to the upper end of the first cylinder, and the other end is sleeved on the outer wall of the third fluid tube 333, thereby locking and fixing the third fluid tube 333, which is usually very convenient to operate.

[0038] It is understandable that in order to better introduce the sample into the sampling chamber 21, in some embodiments of the present invention, the end of the third fluid tube 333 that is away from the first three-way connector 321 extends into the sampling chamber 21, and the outlet end of the third fluid tube 333 is close to the outlet end of the sampling chamber 21, so that the sample can be fully introduced into the sampling chamber 21 through the third fluid tube 333.

[0039] It is understandable that, in order to facilitate the connection between the lower end of the first cylinder and the inlet end of the second stop valve 312, in some embodiments of the present utility model, the heat exchange assembly 2 further includes a second ferrule joint 342, one end of the second ferrule joint 342 is connected to the lower end of the first cylinder, and the other end is connected to the inlet end of the second stop valve 312 through the fifth fluid pipe 335, so that when the liquid sample flows out of the sampling cavity 21, it can pass through the fifth fluid pipe 335 and enter the second stop valve 312 to prevent leakage of the liquid sample. Of course, by controlling the opening of the second stop valve 312, the sampling and collection of the liquid sample can be controlled.

[0040] The embodiments of the present invention are described in detail above in conjunction with the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge scope of ordinary technicians in the relevant technical field without departing from the purpose of the present invention.

Claims

1. A hydrothermal high-pressure reactor in-situ quantitative sampling device, characterized in that: include: A heat exchange component, wherein the heat exchange component has a sampling cavity and a heat exchange cavity, and the heat in the sampling cavity can be transferred to the heat exchange cavity; A fluid pipeline assembly, wherein the fluid pipeline assembly is provided with a first stop valve and a second stop valve, wherein the inlet end of the first stop valve is connected to the outlet end of the hydrothermal high-pressure reactor, the outlet end of the first stop valve is connected to the inlet end of the sampling chamber, and the inlet end of the second stop valve is connected to the outlet end of the sampling chamber.

2. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 1, characterized in that: The heat exchange assembly is provided with a first cylinder and a second cylinder. The second cylinder is arranged outside the first cylinder. The inner cavity of the first cylinder constitutes the sampling cavity. The cavity formed by the second cylinder and the first cylinder constitutes the heat exchange cavity.

3. The in-situ quantitative sampling device for the hydrothermal high-pressure reactor according to claim 2, characterized in that: The second cylinder is connected to a first cooling tube and a second cooling tube, the first cooling tube is used to input cooling liquid into the heat exchange cavity, and the second cooling tube is used to discharge the cooling liquid in the heat exchange cavity.

4. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 3, characterized in that: The first cooling pipe is connected to the outer side wall of the lower end of the second cylinder, and the second cooling pipe is connected to the outer side wall of the upper end of the second cylinder.

5. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 3, characterized in that: An anti-slip structure is provided at the end of the first cooling tube and / or the second cooling tube away from the second cylinder.

6. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to any one of claims 2 to 5, characterized in that: The sampling device also includes a pressure gauge, and the fluid pipeline assembly is also provided with a first three-way joint, a second three-way joint and a third stop valve, the outlet end of the first stop valve is connected to the inlet end of the first three-way joint through a first fluid pipe, one of the outlet ends of the first three-way joint is connected to the inlet end of the second three-way joint through a second fluid pipe, the other outlet end of the first three-way joint is connected to the sampling chamber through a third fluid pipe, the pressure gauge is connected to one of the outlet ends of the second three-way joint, and the inlet end of the third stop valve is connected to the other outlet end of the second three-way joint through a fourth fluid pipe.

7. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 6, characterized in that: The first three-way connector and the second three-way connector are both ferrule-type three-way connectors, and the first stop valve, the second stop valve and the third stop valve are all ferrule-type stop valves.

8. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 6, characterized in that: The heat exchange assembly also includes a first ferrule joint, one end of which is connected to the upper end of the first cylinder, and the other end of which is sleeved on the outer wall of the third fluid pipe.

9. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 8, characterized in that: One end of the third fluid tube away from the first three-way connector extends into the sampling cavity, and the outlet end of the third fluid tube is close to the outlet end of the sampling cavity.

10. The in-situ quantitative sampling device for a hydrothermal high-pressure reactor according to claim 6, characterized in that: The heat exchange assembly also includes a second ferrule joint, one end of which is connected to the lower end of the first cylinder, and the other end of which is connected to the inlet end of the second stop valve through a fifth fluid pipe.

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