High-temperature and high-pressure reaction kettle online sampling device adaptive to hydrothermal conversion of biomass platform compound and detection method of high-temperature and high-pressure reaction kettle online sampling device
By designing an online sampling device for high-temperature and high-pressure reactors that are adapted to hydrothermal conversion of biomass platform compounds, the problems of sampling accuracy and comprehensive detection in the prior art are solved, and accurate sampling and all-round detection under high temperature and high pressure conditions are achieved.
Patent Information
- Application Number
- CN202411710815.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-27
- Publication Date
- 2025-03-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing online sampling device for high-temperature and high-pressure reactors has problems such as low temperature, difficult to accurately control the sampling volume and rate, insufficient comprehensive sample detection, and inability to achieve sample reflux in high-temperature and high-pressure states.
An online sampling device for high-temperature and automatic pressure reactors including a reactor stand, a magnetic stirring device, a sampling device and a spectroscopic detection device is designed. The device uses stainless steel sampling tubes and gear pumps for precise control sampling, uses optical microporous sampling panels and light shields for all-round information detection, and reduces sampling interference through the sample return structure.
It realizes precise control of sampling volume and time under high temperature and high pressure conditions, ensures comprehensiveness and accuracy of detection, and reduces the impact of sample extraction on reaction equilibrium.
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Figure CN119574213A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of online sampling devices for high-temperature and high-pressure reactors, and in particular to an online sampling device for high-temperature and high-pressure reactors adapted for hydrothermal conversion of biomass platform compounds and a detection method thereof. Background Art
[0002] The utilization of biomass resources and energy has great development potential. The main way to utilize biomass is to convert biomass into conventional solid, liquid and gaseous fuels and various chemicals through fermentation, combustion, gasification, pyrolysis, hydrothermal conversion and baking. Among them, hydrothermal conversion technology is a process of converting biomass into renewable energy or high-value-added chemicals under high-temperature and high-pressure water environment. Its principle is mainly that the organic components in the waste are dissolved, reacted and rearranged in high-temperature and high-pressure water under hydrothermal conditions to produce liquid fuels, gases or compounds that can be used as chemical raw materials. However, due to the high complexity of biomass and hydrothermal conversion processes, the quality of biomass hydrothermal conversion products is difficult to control, which limits its application. In order to achieve product selectivity control, biomass platform compounds are widely used as reactant raw materials. These compounds have gained widespread attention in the current promotion of environmental protection and sustainable development due to their green, environmentally friendly, renewable and biodegradable properties. However, the unclear hydrothermal conversion process is still a bottleneck problem in the utilization of biomass hydrothermal conversion technology.
[0003] High-temperature and high-pressure hydrothermal reactors are the most common biomass hydrothermal conversion reactors. However, due to the high-temperature and high-pressure hydrothermal reaction conditions, the conversion process of biomass in hydrothermal reactors is unknown. The study of the reaction mechanism in a pressurized closed container at high temperature is a major challenge. Nowadays, people mainly use intermittent operations to clarify the characteristics of raw materials and products before and after the reaction, and cannot understand the reaction process in real time.
[0004] In view of this, the development of an online sampling device for a high-temperature and high-pressure reactor suitable for the hydrothermal conversion of biomass platform compounds is of great significance for the exploration of the complex biomass hydrothermal conversion reaction process.
[0005] The current online sampling of biomass platform compounds in high temperature and high pressure reactors faces the following problems:
[0006] (1) The applicable temperature is low (<180°C). The sampling equipment of the high temperature and high pressure reactor must be able to withstand the high temperature and high pressure inside the reactor while ensuring good sealing of the sampling system.
[0007] (2) It is impossible to accurately control the sampling volume and sampling rate, and it is impossible to ensure long-term continuous sampling. The commonly used intermittent sampling will take out a large amount of liquid at one time due to the huge pressure difference, causing the pressure in the kettle to drop sharply. The sampling system needs to be operated accurately and respond quickly to ensure the continuity of sampling.
[0008] (3) The comprehensiveness of sample testing cannot be guaranteed. When conducting online spectroscopy analysis, a large amount of sample liquid accumulation will affect the comprehensiveness of the test. During the test process, it is necessary to use a small amount of sample liquid to perform the most comprehensive test.
[0009] (4) It is impossible to achieve sample reflux under high temperature and high pressure. Due to the high pressure in the kettle, it is difficult to achieve reflux of the sample after removal. The removal of a large amount of sample will cause the liquid and pressure in the kettle to decrease rapidly, and the gas-liquid equilibrium and chemical reaction equilibrium will change.
[0010] In order to timely, efficiently and accurately explore the hydrothermal conversion reaction process, it is necessary to provide a new type of reactor online sampling device and its detection method, which can meet the needs of high temperature and high pressure conditions, accurately control the sampling volume and sampling time, conduct all-round information detection of samples, realize reflux and reduce sampling interference, so as to reveal the process of biomass hydrothermal conversion reaction. Summary of the invention
[0011] The main purpose of the present invention is to provide an online sampling device for a high-temperature and high-pressure reactor suitable for hydrothermal conversion of biomass platform compounds and a detection method thereof, so as to solve the problems existing in the prior art.
[0012] In order to solve the above technical problems, the present invention adopts the following technical solutions:
[0013] A high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds, comprising:
[0014] A reactor rack, on which a reactor is arranged;
[0015] A magnetic stirring device, which is connected to the reactor frame and is used to stir the interior of the reactor;
[0016] A sampling device, which is arranged at one side of the reactor and connected to the inside of the reactor, and is used for sampling and returning samples from the inside of the reactor;
[0017] A spectroscopic detection device is connected to the sampling device, and is used for performing spectroscopic detection on the sample.
[0018] Furthermore, the magnetic stirring device includes a magnetic transmission coupling and a stirring paddle, the magnetic transmission coupling is connected to the reactor frame and arranged at the top of the reactor, the magnetic transmission coupling is connected to the top of the stirring paddle, and the other end of the stirring paddle extends to the interior of the reactor body.
[0019] Furthermore, the sampling device includes a sampling bottom probe needle, a high-pressure sampling needle valve, a stainless steel sampling tube, a three-way valve, a sampling gear pump, a return sample gear pump, a stainless steel return sample tube, a high-pressure return sample needle valve and a return sample bottom probe needle. The high-pressure sampling needle valve and the high-pressure return sample needle valve are both connected to the top of the reactor, one end of the high-pressure sampling needle valve extends to the interior of the reactor and is connected to the sampling bottom probe needle, one end of the high-pressure return sample needle valve extends to the interior of the reactor and is connected to the return sample bottom probe needle, one end of the sampling bottom probe needle and the return sample bottom probe needle both extend to the bottom end of the reactor, the end of the high-pressure sampling needle valve away from the sampling bottom probe needle is sequentially connected to the stainless steel sampling tube, the three-way valve, the spectroscopy monitoring device, the stainless steel return sample tube and the high-pressure return sample needle valve, the sampling gear pump is connected to the stainless steel sampling tube, the return sample gear pump is connected to the stainless steel return sample tube, and the sampling gear pump and the return sample gear pump are both connected to a stepping motor.
[0020] Furthermore, the bottom end of the sampling probe, the bottom end of the return sample probe, and the blade of the stirring paddle are in the same horizontal plane, and the spacing between the sampling probe and the blade of the stirring paddle, and between the return sample probe and the blade of the stirring paddle is 1cm-2cm.
[0021] Furthermore, a sampling pipe is arranged inside the valve body of the high-pressure sampling needle valve, the valve body is connected to the valve cap through a joint nut, an adjusting valve stem and a connecting pipe are arranged inside the valve cap, a sealing gasket is arranged at the interface between the valve body and the valve cap, a locking nut and a packing gland nut are arranged outside the valve bonnet, an internal thread is arranged on the inner wall of the packing gland nut, an external thread is arranged on the outer wall of the adjusting valve stem, the packing gland nut is threadedly connected to the adjusting valve stem, and a handle is arranged on the top of the adjusting valve stem.
[0022] Furthermore, the stainless steel sampling tube includes a sampling tube body and a sealing gasket. The inner wall of the sampling tube body is smooth and free of burrs. The sampling tube body is provided with an external thread. The sampling gear pump is provided with an internal thread. The sampling tube body is threadedly connected to the sampling gear pump, and the sealing gasket is provided at the threaded connection.
[0023] Furthermore, the other two ends of the three-way valve that are not connected to the stainless steel sampling tube are respectively connected to a spectroscopy detection device and an invasive analysis device.
[0024] Furthermore, the spectroscopy detection device includes an optical microporous sampling plate and a light shield, the optical microporous sampling plate is connected to the sampling device, and the light shield is arranged on the outer peripheral side of the optical microporous sampling plate.
[0025] Furthermore, the optical microporous sampling plate includes a plurality of parallel capillary channel structures, and the plurality of parallel capillary channel structures are connected to form a glass plate, and the formed glass plate is connected to the sampling device.
[0026] A high-temperature and high-pressure reactor online sampling and detection method adapted for hydrothermal conversion of biomass platform compounds, using a high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds, comprising the following steps:
[0027] S1: Perform sampling operation and adjust the three-way valve behind the sampling gear pump to allow the sample to flow to the bottom opening of the optical microporous sampling plate;
[0028] S2: After entering the optical microporous sampling plate, the sample is slowly and evenly filled into the entire optical microporous sampling plate through the capillary action of the capillary channel structure in the optical microporous sampling plate;
[0029] S3: Use a spectrum analyzer to spectrally irradiate the optical micropore sampling plate and the internal samples inside the light shield;
[0030] S4: Filter the spectrum generated by the optical microporous sampling plate itself according to the data of the optical microporous sampling plate to obtain a pure sample spectrum.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] 1. The sampling system of the online sampling device of the high-temperature and high-pressure reactor adapted for the hydrothermal conversion of biomass platform compounds is designed. The sampling gear pump connected by the stainless steel sampling tube samples the samples in the reactor, which can accurately control the sampling amount and sampling time, and effectively control the sampling rate.
[0033] 2. Design an optical microporous sampling plate, and use the capillary action of the capillary channel structure to evenly spread the sample liquid on a two-dimensional plane that is as thin as possible, effectively reducing the demand for sample liquid and ensuring the comprehensiveness and accuracy of the test.
[0034] 3. Design a light shield to effectively block the influence of external light sources on spectroscopy detection results.
[0035] 4. The designed sampling device also includes a sample return structure, which effectively reduces the impact of sample removal on the original reaction balance.
[0036] 5. The device is easy to operate, occupies a small area, can be used under high temperature and high pressure conditions, can accurately control the sampling volume and sampling time, conduct all-round information detection of samples, and achieve reflux to reduce sampling interference. It can safely monitor the hydrothermal reaction state in real time, ensure the safety of operation, and lay a good foundation for optimizing process system control. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] Figure 1 It is an overall schematic diagram of an online sampling device for a high-temperature and high-pressure reactor suitable for hydrothermal conversion of biomass platform compounds according to the present invention.
[0038] Figure 2 Another overall schematic diagram of an online sampling device for a high-temperature and high-pressure reactor adapted for hydrothermal conversion of biomass platform compounds according to the present invention;
[0039] Figure 3 for Figure 2 A partial enlarged view of
[0040] Figure 4 It is a schematic diagram of the optical microporous sampling plate in the spectroscopy detection device of the present invention.
[0041] Among them, 1-reaction kettle frame; 2-magnetic stirring device; 21-magnetic transmission coupling; 22-stirring paddle; 3-sampling device; 31-sampling bottom probe; 32-high-pressure sampling needle valve; 33-stainless steel sampling tube; 34-three-way valve; 35-sampling gear pump; 36-return sample gear pump; 37-stainless steel return sample tube; 38-high-pressure return sample needle valve; 39-return sample bottom probe; 4-spectroscopy detection device; 41-optical microporous sampling plate; 411-capillary channel structure; 42-light shield; 5-stepping motor; 6-heating coil; 7-intrusive detection equipment sampling tube; 8-spectroscopy detection equipment sampling tube. DETAILED DESCRIPTION
[0042] The technical solution of the present invention is further described below through the accompanying drawings and embodiments.
[0043] Example 1
[0044] Combination Figure 1-4 The present invention provides an online sampling device for a high-temperature and high-pressure reactor suitable for hydrothermal conversion of biomass platform compounds, comprising a reactor frame 1, a magnetic stirring device 2, a sampling device 3, a spectroscopic detection device 4 and a sensor device. A reactor (not shown in the figure) is arranged on the reactor frame 1, and the reactor comprises a reactor body, and a reactor cavity is formed inside the reactor body. The magnetic stirring device 2 is connected to the reactor frame 1 and is used for stirring the inside of the reactor. The sampling device 3 is arranged on one side of the reactor and connected to the inside of the reactor, and is used for sampling and returning the inside of the reactor. The spectroscopic detection device 4 is connected to the sampling device 3, and the spectroscopic detection device 4 is used for spectroscopic detection of the sample.
[0045] In this embodiment, the reaction kettle frame 1 provides support for the reaction kettle, the magnetic stirring device 2, the sampling device 3, and the sensor device.
[0046] The magnetic stirring device 2 includes a magnetic transmission coupling 21 and a stirring paddle 22. The magnetic transmission coupling 21 is connected to the top of the reactor frame 1 and is arranged at the top of the reactor. The magnetic transmission coupling 21 is connected to the top of the stirring paddle 22 through the mounting port on the reactor frame 1, and the other end of the stirring paddle 22 extends to the inside of the reactor body.
[0047] The sampling device 3 includes a sampling bottom probe needle 31, a high-pressure sampling needle valve 32, a stainless steel sampling tube 33, a three-way valve 34, a sampling gear pump 35, a return sample gear pump 36, a stainless steel return sample tube 37, a high-pressure return sample needle valve 38 and a return sample bottom probe needle 39. The high-pressure sampling needle valve 32 and the high-pressure return sample needle valve 38 are both connected to the top of the reactor, one end of the high-pressure sampling needle valve 32 extends to the interior of the reactor and is connected to the sampling bottom probe needle 31, and one end of the high-pressure return sample needle valve 38 extends to the reactor. The interior of the reactor is connected to the return sample bottom probe needle 39, and one end of the sampling bottom probe needle 31 and the return sample bottom probe needle 39 both extend to the bottom end of the interior of the reactor. The end of the high-pressure sampling needle valve 32 away from the sampling bottom probe needle 31 is sequentially connected to a stainless steel sampling tube 33, a three-way valve 34, a spectroscopy monitoring device 4, a stainless steel return sample tube 37 and a high-pressure return sample needle valve 38. The sampling gear pump 35 is connected to the stainless steel sampling tube 33, and the return sample gear pump 36 is connected to the stainless steel return sample tube 37.
[0048] The sampling gear pump 35 and the return sample gear pump 36 are both connected to a stepper motor 5. In this embodiment, the rotation speeds of the two gear pumps are controlled by controlling the pulse frequency of the stepper motor 5 to achieve the effect of controlling the sampling flow rate and accurately controlling the sampling volume and sampling time.
[0049] The three-way valve 34 controls the sample flow channel through the diverter valve to selectively pass the sample into the required detection equipment: the sample is passed into the invasive detection equipment through the invasive detection equipment sampling tube 7, and the sample is passed into the optical microporous sampling plate 41 through the spectroscopy detection equipment sampling tube 8. After completing the spectroscopy detection, the sample is pumped by the return gear pump 36 through the stainless steel return tube 37, the high-pressure return needle valve 38 and the return bottom needle 39 and returned to the reactor.
[0050] In this embodiment, a sampling bottom probe 31 , a return sample bottom probe 39 , a heating coil 6 and a stirring paddle 22 are arranged inside the reactor chamber.
[0051] The bottom end of the sampling probe 31, the bottom end of the return sample probe 39, and the blades of the stirring paddle 22 are in the same horizontal plane, and the minimum spacing (the distance between the close ends) between the sampling probe 31 and the blades of the stirring paddle 22, and between the return sample probe 39 and the blades of the stirring paddle 22 is 1cm-2cm.
[0052] A sampling pipeline is arranged inside the valve body of the high-pressure sampling needle valve 32, and the valve body is connected to the valve cap through a joint nut. An adjusting valve stem and a connecting pipe are arranged inside the valve cap. A sealing gasket is arranged at the interface between the valve body and the valve cap. A locking nut and a packing gland nut are arranged outside the valve bonnet to ensure the sealing of the high-pressure sampling needle valve. An internal thread is arranged on the inner wall of the packing gland nut, and an external thread is arranged on the outer wall of the adjusting valve stem. The packing gland nut is threadedly connected to the adjusting valve stem, and a handle is arranged on the top of the adjusting valve stem.
[0053] The stainless steel sampling tube 33 includes a sampling tube body and a sealing gasket. The inner wall of the sampling tube body is smooth and burr-free. The sampling tube body is provided with an external thread. The sampling gear pump 35 is provided with an internal thread. The sampling tube body is threadedly connected to the sampling gear pump 35, and the sealing gasket is provided at the threaded connection.
[0054] The other two ends of the three-way valve 34 that are not connected to the stainless steel sampling tube 33 are respectively connected to a spectroscopy detection device 4 and an invasive analysis device.
[0055] The spectroscopy detection device 4 includes an optical microporous sampling plate 41 and a light shield 42. The optical microporous sampling plate 41 is connected to the sampling device 3. The light shield 42 is arranged on the outer peripheral side of the optical microporous sampling plate 41 to eliminate the influence of external light sources on the detection results.
[0056] In some other embodiments, the light shield 42 may be a box structure with a hinged door disposed on one side.
[0057] The optical microporous sampling plate 41 includes a plurality of parallel capillary channel structures 411 . The plurality of parallel capillary channel structures 411 are connected to form a glass plate, and the formed glass plate is connected to the sampling device 3 .
[0058] The sampling tube 8 of the spectroscopy detection device is connected to the bottom of the optical microporous sampling plate 41, which is arranged outside the reactor and embedded in the sampling device 3. The optical microporous sampling plate 41 contains a plurality of parallel precise capillary channel structures 411, such as Figure 4 As shown. When the sample is introduced from the bottom of the optical microporous sampling plate 41, due to the capillary action, a small amount of solution sample can be evenly filled in the glass plate, ensuring uniform sampling and paving, which is conducive to the comprehensive detection of the sample. The top of the optical microporous sampling plate 41 is connected to the stainless steel sample return tube 37, and the sample taken out is returned to the inside of the reactor through the sample return gear pump 36 to achieve sample return. The returned sample can continue to participate in the reaction, reducing the impact of the material reduction on the reaction system process.
[0059] More specifically, when conducting a hydrothermal conversion reaction experiment, the system in the reactor is divided into a homogeneous system and a heterogeneous system. The heterogeneous system contains at least two phases, of which the solid-liquid two-phase system occupies the majority, and the reaction raw materials, catalysts, etc. may exist as solid phases in the reaction system.
[0060] Developing efficient catalysts and reaction systems to improve the yield and selectivity of hydrothermal conversion reactions may be the future research focus of hydrothermal conversion technology. Among them, solid heterogeneous catalysts have many advantages such as high selectivity, good thermal stability, environmental friendliness, wide application range, rich active sites, large surface area, easy separation and recovery, and reusability. They occupy an important position in the modern chemical industry and play a key role in promoting green chemistry and dual carbon goals and sustainable development. The solid heterogeneous catalysts used in the hydrothermal conversion process mainly include metal catalysts such as precious metals and transition metals, metal oxide catalysts, molecular sieve catalysts such as zeolite molecular sieves and metal organic frameworks (MOFs), solid acid catalysts such as proton-type and Lewis acids, solid base catalysts, carbon material catalysts, nanocatalysts, biocatalysts, semiconductor photocatalysts and electrode material electrocatalysts, etc. The specific particle size of solid heterogeneous catalysts can be controlled by the catalyst preparation process.
[0061] The suspension containing solid particles with larger particle size is directly transformed into a mixed solution of small solid particles with a solid particle diameter of ≤400 mesh (38 μm) by the sampling gear pump 35, and can smoothly pass through the optical microporous sampling plate 41. When the capillary channel structure 411 in the optical microporous sampling plate 41 detects the sample after passing through the gear pump, the wavelength of the catalyst and the optical microporous sampling plate 41 itself can be filtered out by Fourier transform and other calculation methods to obtain the reactant state detection result.
[0062] like Figure 4 As shown, the glass plate formed by the optical microporous sampling plate 41 is closed on all sides, and the openings in the middle of the upper and lower ends are connected to the stainless steel sampling tube 33 and the stainless steel return sample tube 37. The openings are provided with internal threads for fixing.
[0063] The inner diameter of the capillary channel structure 411 of the optical microporous sampling plate 41 of the present invention is 10μm-200μm, preferably 100μm, and the thickness of the sampling plate is 30μm-300μm, preferably 165μm. In some other embodiments, the specific size can be customized according to the requirements of the reaction system.
[0064] When the present invention is put into practical application, a necked butt-welded flange (not shown in the figure) is arranged on the top of the reactor, and the flange plate and the flange cover are connected by studs and nuts or fastened by clamping rings and corresponding bolts; the reactor is equipped with a heating coil, a heating and heat-insulating sleeve, a lifting slide and a rotating shaft, etc.; the working principle of the heating coil 6 is to heat the heat-conducting oil with electrical energy through a resistance wire to convert it into thermal energy, thereby heating the reactor cavity through heat transfer, and a heat-insulating foam is arranged in the heating and heat-insulating sleeve to reduce heat loss during the heating process.
[0065] As an optimization, a cooling water circulation pipeline is set inside the reactor (not shown in the figure). The outside of the cooling water circulation pipeline is divided into a water inlet and a water outlet, which is connected to the water tank through two rubber tubes. A U-shaped cooling pipe is set in the reactor cavity, and the U-shaped cooling pipe extends to the bottom of the reactor.
[0066] As an optimization, the temperature, pressure control and monitoring of the hydrothermal conversion reaction are controlled by an external programmable temperature controller (not shown in the figure), and the programmable temperature controller is connected to the heating layer and the reactor through temperature sensors and pressure sensors respectively.
[0067] As an optimization, the reactor is provided with a temperature sensor probe installation port, a pressure sensor probe installation port and a dielectric constant test probe installation port (not shown in the figure), that is, a pressure sensor, a temperature sensor and a dielectric constant tester are installed on the reactor to monitor various parameters of the reaction products in the reactor in real time.
[0068] In this embodiment, the designed maximum temperature of the reactor is 450° C., and the designed maximum pressure is 35 MPa.
[0069] When the device is running, after the hydrothermal conversion reaction in the reactor cavity is completed, the program temperature controller controls the heating coil and the heating insulation jacket to stop heating, and the heating insulation jacket is opened to quickly cool the reactor. When the temperature in the reactor drops to room temperature, the gas in the reactor is collected through the gas outlet provided by the high-pressure sampling needle valve 32. When the pressure in the reactor is close to the ambient pressure, the reactor is opened, and the materials after the reaction are taken out with the reactor body, and the bio-oil or chemical liquid phase products and solid products are subjected to subsequent product separation and storage treatment.
[0070] Example 2
[0071] A high-temperature and high-pressure reactor online sampling and detection method adapted for hydrothermal conversion of biomass platform compounds, using a high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds, comprising the following steps:
[0072] S1: Perform sampling operation and adjust the three-way valve 34 behind the sampling gear pump to allow the sample to flow to the bottom opening of the optical microporous sampling plate 41 .
[0073] S2: After entering the optical microporous sampling plate 41 , the sample is slowly and evenly filled into the entire optical microporous sampling plate through the capillary action of the capillary channel structure in the optical microporous sampling plate 41 .
[0074] S3: Use a spectrum analyzer to spectrally illuminate the optical micropore sampling plate and the internal samples inside the light shield.
[0075] S4: Filter the spectrum generated by the optical microporous sampling plate itself according to the data of the optical microporous sampling plate (material, thickness, capillary channel structure diameter, etc.), so as to obtain a pure sample spectrum.
[0076] When the sampling device is in operation, the stepping motor 5 and the two gear pumps are controlled to operate so as to take out the sample from the reaction kettle or to transfer the sample from the spectroscopy detection device 4 back.
[0077] The above description is only a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any slight modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.
Claims
1. A high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds, characterized in that: include: A reactor rack, on which a reactor is arranged; A magnetic stirring device, which is connected to the reactor frame and is used to stir the interior of the reactor; A sampling device, which is arranged at one side of the reactor and connected to the inside of the reactor, and is used for sampling and returning samples from the inside of the reactor; A spectroscopic detection device is connected to the sampling device, and is used for performing spectroscopic detection on the sample.
2. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 1, characterized in that: The magnetic stirring device includes a magnetic transmission coupling and a stirring paddle. The magnetic transmission coupling is connected to the reactor frame and arranged at the top of the reactor. The magnetic transmission coupling is connected to the top of the stirring paddle, and the other end of the stirring paddle extends to the inside of the reactor body.
3. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 2, characterized in that: The sampling device includes a sampling bottom probe needle, a high-pressure sampling needle valve, a stainless steel sampling tube, a three-way valve, a sampling gear pump, a return sample gear pump, a stainless steel return sample tube, a high-pressure return sample needle valve and a return sample bottom probe needle. The high-pressure sampling needle valve and the high-pressure return sample needle valve are both connected to the top of the reactor. One end of the high-pressure sampling needle valve extends to the interior of the reactor and is connected to the sampling bottom probe needle. One end of the high-pressure return sample needle valve extends to the interior of the reactor and is connected to the return sample bottom probe needle. One end of the sampling bottom probe needle and the return sample bottom probe needle both extend to the inner bottom end of the reactor. The end of the high-pressure sampling needle valve away from the sampling bottom probe needle is sequentially connected to the stainless steel sampling tube, the three-way valve, the spectroscopy monitoring device, the stainless steel return sample tube and the high-pressure return sample needle valve. The sampling gear pump is connected to the stainless steel sampling tube, the return sample gear pump is connected to the stainless steel return sample tube, and the sampling gear pump and the return sample gear pump are both connected to a stepping motor.
4. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds as claimed in claim 3, characterized in that: The bottom end of the sampling probe needle, the bottom end of the return sample probe needle, and the blade of the stirring paddle are in the same horizontal plane, and the spacing between the sampling probe needle and the blade of the stirring paddle, and between the return sample probe needle and the blade of the stirring paddle is 1cm-2cm.
5. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 3, characterized in that: A sampling pipeline is arranged inside the valve body of the high-pressure sampling needle valve, and the valve body is connected to the valve cap through a joint nut. An adjusting valve stem and a connecting pipe are arranged inside the valve cap. A sealing gasket is arranged at the interface between the valve body and the valve cap. A locking nut and a packing gland nut are arranged outside the valve bonnet. An internal thread is arranged on the inner wall of the packing gland nut, and an external thread is arranged on the outer wall of the adjusting valve stem. The packing gland nut is threadedly connected to the adjusting valve stem, and a handle is arranged on the top of the adjusting valve stem.
6. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 3, characterized in that: The stainless steel sampling tube comprises a sampling tube body and a sealing gasket. The inner wall of the sampling tube body is smooth and free of burrs. The sampling tube body is provided with an external thread. The sampling gear pump is provided with an internal thread. The sampling tube body is threadedly connected to the sampling gear pump, and the sealing gasket is provided at the threaded connection.
7. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 3, characterized in that: The other two ends of the three-way valve that are not connected to the stainless steel sampling tube are respectively connected to a spectroscopy detection device and an invasive analysis device.
8. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 2, characterized in that: The spectroscopy detection device comprises an optical microporous sampling plate and a light shield. The optical microporous sampling plate is connected to the sampling device, and the light shield is arranged on the outer peripheral side of the optical microporous sampling plate.
9. The high-temperature and high-pressure reactor online sampling device adapted for hydrothermal conversion of biomass platform compounds according to claim 8, characterized in that: The optical microporous sampling plate comprises a plurality of parallel capillary channel structures, and the plurality of parallel capillary channel structures are connected to form a glass plate, and the formed glass plate is connected to a sampling device.
10. An online sampling and detection method for a high-temperature and high-pressure reactor suitable for hydrothermal conversion of a biomass platform compound, using the online sampling device for a high-temperature and high-pressure reactor suitable for hydrothermal conversion of a biomass platform compound according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1: Perform sampling operation and adjust the three-way valve behind the sampling gear pump to allow the sample to flow to the bottom opening of the optical microporous sampling plate; S2: After entering the optical microporous sampling plate, the sample is slowly and evenly filled into the entire optical microporous sampling plate through the capillary action of the capillary channel structure in the optical microporous sampling plate; S3: Use a spectrum analyzer to spectrally irradiate the optical micropore sampling plate and the internal samples inside the light shield; S4: Filter the spectrum generated by the optical microporous sampling plate itself according to the data of the optical microporous sampling plate to obtain a pure sample spectrum.