Dynamic adsorption detection method and equipment for adsorbent

Abstract

The invention relates to an adsorbent dynamic adsorption detection method and equipment thereof, and the method comprises the following steps: carrying out regeneration treatment on an adsorbent to obtain a regenerated adsorbent; adjusting the temperature of the constant-temperature water bath according to the required test temperature; weighing the regeneration adsorbent with the specified weight, putting into an adsorption device, and sealing; starting an air compressor to output an air source, adjusting the pressure and the flow to a test range, and continuously conveying a constant-temperature air source to the adsorption device after the air source passes through the constant-temperature water bath; the dew point of the adsorption device is observed, when the dew point reaches a set threshold value, the air compressor is closed, and conveying of the air source is stopped; and after the pressure is reduced to 0 Mpa, opening the adsorption device, taking out the adsorbed adsorbent, weighing the weight of the adsorbent after adsorption to obtain the adsorption capacity of the adsorbent, and judging the adsorption performance of the adsorbent according to the adsorption capacity. The method has the effects of shortening the detection time and improving the detection efficiency.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of adsorbents, in particular to a dynamic adsorption detection method and device for adsorbents. BACKGROUND

[0002] Adsorption separation technology is one of the core unit operations in the fields of chemical industry, environmental protection, energy, medical treatment and the like, and its efficiency is highly dependent on the performance of the adsorbent material itself. Nowadays, there are more and more manufacturers producing adsorbents on the market, and the variety of adsorbents has also increased accordingly. Different operating conditions in different industries require different adsorbent performances, and therefore it is usually necessary to understand the actual adsorption performance of various adsorbents. The existing method for judging the adsorption performance of adsorbents usually adopts a static test method, in which the adsorbent is allowed to contact with the adsorbate in a closed system until the system reaches thermodynamic equilibrium, and the entire process may take several hours to several days. In addition, static adsorption only represents the saturated adsorption amount of the adsorbent to the adsorbate, but the performance of the adsorbent is not constant, and it is affected by multiple factors such as inlet medium pressure, temperature, flow rate and the like. Static adsorption is difficult to simulate various operating conditions such as temperature variation, pressure variation, complex mixed gas, humidity control and the like. Therefore, another adsorbent performance detection method is needed to detect the actual adsorption performance under different operating conditions, so as to shorten the detection time. SUMMARY

[0003] In view of this, the present application provides a dynamic adsorption detection method and device for adsorbents to dynamically test the actual performance of the adsorbents according to different operating conditions.

[0004] In one aspect, the present application provides a dynamic adsorption detection method for adsorbents, which adopts the following technical solution: A dynamic adsorption detection method for adsorbents, comprising the steps of: regenerating the adsorbent to obtain a regenerated adsorbent; adjusting the temperature of the constant-temperature water bath according to the required test temperature; weighing a specified amount of the regenerated adsorbent and placing it into an adsorption device and sealing it; starting an air compressor to output a gas source, adjusting the pressure and flow rate to the test range, and allowing the gas source to continuously transport a constant-temperature gas source to the adsorption device after passing through the constant-temperature water bath; observing the dew point of the adsorption device, and closing the air compressor and stopping the transportation of the gas source when the dew point reaches a set threshold value; opening the adsorption device after the pressure drop is 0 Mpa, taking out the adsorbed adsorbent and weighing its weight after adsorption to obtain the adsorption amount of the adsorbent, and judging the adsorption performance of the adsorbent according to the adsorption amount.

[0005] By adopting the technical scheme, the detection time can be shortened, and the working conditions of different temperatures, pressures and flow rates can be simulated for testing, so that the detection efficiency and reliability are improved.

[0006] Preferably, the step of regenerating the adsorbent includes: The first container is placed on the weighing platform to zero, and the adsorbent is put into the first container according to the detection requirement. The first container and the adsorbent are put into the vacuum drying box for heating and drying. After reaching the set heating time, the vacuum drying box is closed and the exhaust valve is opened for pressure relief. After the pressure relief is completed, the first container and the adsorbent are taken out and quickly placed in a dry dish for cooling. After cooling, the regenerated adsorbent is obtained.

[0007] By adopting the technical scheme, the adsorbent is regenerated before testing, so that the adsorbent is tested in the original state, and the test effect can be avoided.

[0008] Preferably, the step of adjusting the temperature of the constant temperature water bath according to the required test temperature includes: Confirming that the water level of the constant temperature water bath is higher than the internal heat exchange pipe, setting the temperature of the constant temperature water bath according to the environmental temperature, adjusting the water bath temperature, and making the actual temperature of the water bath within the set temperature difference threshold.

[0009] By adopting the technical scheme, the constant temperature gas source can be obtained according to different working condition requirements, so that the gas source maintains the same temperature during testing, thereby improving the stability and reliability of the test.

[0010] Preferably, the step of weighing the regenerated adsorbent and placing it in the adsorption device and closing it includes: Recording the temperature and humidity of the experimental environment and the actual time; Opening the recorder and flowmeter of the adsorption device, and in the case that the recorder time is consistent with the actual time, opening the feed inlet of the adsorption device and sleeving the funnel; Weighing the regenerated adsorbent, and pouring the regenerated adsorbent into the adsorption device through the funnel; Covering the feed inlet and closing it.

[0011] By adopting the technical scheme, the test data can be recorded for subsequent analysis.

[0012] Preferably, the step of taking out the adsorbed adsorbent and weighing the weight of the adsorbed adsorbent includes: The second container is weighed to zero, the adsorption device is opened, the internal adsorbent is taken out, the weight of the adsorbed adsorbent is weighed, and the volume of the second container is greater than that of the first container.

[0013] By adopting the above technical scheme, the larger second container can accommodate the adsorbent after adsorption, facilitating weighing, and judging the adsorption performance by the weight after adsorption, which is simple and intuitive, and improves the detection efficiency.

[0014] On the other hand, the application also provides a kind of adsorbent dynamic adsorption detection equipment, including regenerator, air compressor, constant temperature water bath device and adsorption device, the regenerator includes vacuum drying machine, the air compressor is communicated with the heat exchange pipe in the constant temperature water bath device, the heat exchange pipe is connected with the adsorption device.

[0015] By adopting the above technical scheme, the above adsorption detection method is realized.

[0016] Preferably, the adsorption device includes a recorder, an adsorption column, a quick end cover, a flow meter, a gas-water separation filter, a dew point detector and a pressure sensor, the recorder is used to record and display the temperature, dew point data and flow and pressure data of the gas source in the adsorption column, the adsorption column is used to accommodate the adsorbent, the quick end cover has two, which are respectively detachably connected with the top and bottom of the adsorption column, the gas-water separation filter is connected with the quick end cover of the bottom of the adsorption column and the pressure sensor, the flow meter is connected with the quick end cover of the top of the adsorption column, and the dew point detector is connected with the flow meter.

[0017] By adopting the above technical scheme, the gas-water separation filter filters the water in the gas source to avoid affecting the test data, the dew point detector detects the dew point data, and the specific structure of the adsorption device is provided so that the adsorbent can be tested.

[0018] Preferably, the adsorption device includes an adsorption column and a quick end cover, the adsorption column includes a plurality of circumferentially distributed quick insertion slots, the quick end cover is provided with a plurality of circumferentially distributed insertion blocks, and the quick insertion slots and the insertion blocks are adapted; the quick insertion slot includes a first slot section and a second slot section, the first slot section is vertically arranged and the top end penetrates, the second slot section extends in the circumferential direction, one end of the second slot section is communicated with the bottom end of the first slot section, and the other end is closed and inclined away from the top end of the first slot section.

[0019] By adopting the above technical scheme, the first slot section realizes the quick insertion of the quick end cover and the adsorption column, and the adsorbent can be quickly closed after entering the adsorption column, avoiding the adsorbent from adsorbing gas before testing, which affects the detection effect, the circumferentially extending second slot section places the axial displacement of the quick end cover, and the inclined arrangement of the other end of the second slot section can make the quick end cover and the adsorption column connect closely.

[0020] Preferably, the adsorption device comprises a plurality of limiting structures, the plurality of limiting structures are uniformly distributed along the circumference of the adsorption column, the limiting structure comprises two first mounting codes, a limiting piece and a second mounting code, the two first mounting codes are connected with the quick end cover, the second mounting code is connected with the adsorption column, the limiting piece is rotatably connected with the two first mounting codes, and the limiting piece is clamped with the second mounting code.

[0021] By adopting the above technical scheme, the circumferential displacement of the quick end cover during the test process is prevented, and the connection stability between the quick end cover and the adsorption column is improved.

[0022] Preferably, the adsorption device comprises a chamber adjusting piece, the chamber adjusting piece is connected with the inside of the adsorption column, and the chamber adjusting piece is used for adjusting the volume in the adsorption column to test different amounts of adsorbents.

[0023] By adopting the above technical scheme, the volume in the adsorption column can be adjusted according to different amounts of adsorbents for testing, thereby saving the overall test time.

[0024] By adopting the adsorbent dynamic adsorption detection method and the equipment provided in the embodiments of the present application, the time for detecting the adsorption performance of the adsorbent can be shortened, various working conditions can be simulated, and the detection efficiency and reliability are improved. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 is a flowchart of an adsorbent dynamic adsorption detection method provided by the embodiments of the present application.

[0026] Figure 2 is a schematic diagram of an adsorbent dynamic adsorption detection equipment provided by the first embodiment of the present application.

[0027] Figure 3 is a three-dimensional schematic diagram of a constant-temperature water bath device provided by the first embodiment of the present application.

[0028] Figures 4 to 5 is a schematic diagram of an adsorption device provided by the first embodiment of the present application.

[0029] Figures 6 to 11 is a schematic diagram of an adsorption column and a quick end cover provided by the second embodiment of the present application.

[0030] Figures 12 to 13 is a schematic diagram of an adsorption column and a quick end cover provided by the third embodiment of the present application.

[0031] Figure 14 is a schematic diagram of an adsorption column provided by the fourth embodiment of the present application.

[0032] Explanation of reference signs: 1, regeneration device; 2, air compressor; 3, constant temperature water bath device; 31, water bath box; 32, heat exchange pipe; 33, inlet; 34, outlet; 4, adsorption device; 41, adsorption column; 42, quick end cover; 421, gas pipe interface; 422, temperature sensor; 43, mounting frame; 44, flow meter; 45, digital display panel; 46, gas-water separation filter; 47, dew point detector; 48, pressure sensor; Adsorption column; 511, quick slot; 5111, first slot section; 5112, second slot section; 52, quick end cover; 521, plug; 522, sealing groove; 523, threaded interface; 525, vertical slot; 53, sealing element; 55, limiting structure; 551, first mounting code; 552, second mounting code; 553, limiting element; 55, cavity dividing element; 551, cavity; 56, pouring cover plate; Adsorption column; 611, first adsorption cavity; 612, second adsorption cavity; 62, quick end cover; 621, gas inlet; 622, gas outlet; 71, adsorption column; 711, bottom plate; 72, adjusting structure; 721, adjusting plate; 722, adjusting screw; 723, sealing gasket, 724, nut; 725, gas inlet channel. DETAILED DESCRIPTION

[0033] In order to more clearly understand the purpose, technical scheme and advantages of the present application, the present application is described and explained below in conjunction with the drawings and embodiments. However, it should be understood by those skilled in the art that the present application can be implemented without these details. In some cases, in order to avoid unnecessary description and make aspects of the present application obscure, well-known methods, processes, systems, components and / or circuits that have been described at a higher level will not be described in detail. It is obvious to those skilled in the art that various changes can be made to the embodiments disclosed in the present application, and the general principles defined in the present application can be applied to other embodiments and application scenarios without deviating from the principles and scope of the present application. Therefore, the present application is not limited to the embodiments shown, but conforms to the broadest scope claimed in the present application.

[0034] It should be noted that the description of these embodiments is used to help understand the present application and does not constitute a limitation of the present application. In addition, the technical features involved in each embodiment of the present application described below can be combined with each other as long as they do not conflict with each other.

[0035] In the description of the present application, the meaning of several is one or more, the meaning of multiple is more than two, greater than, less than, more than, etc. are understood as not including the number, above, below, within, etc. are understood as including the number. If it is described as first, second, it is only used to distinguish the technical features for the purpose, and cannot be understood as indicating or implying the relative importance or implicitly indicating the number of indicated technical features or implicitly indicating the sequence of indicated technical features.

[0036] In the description of the present application, the description of the terms "one embodiment", "some embodiments", "exemplary embodiment", "example", "specific example", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In the description, the description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the described specific features, structures, materials or characteristics can be combined in any one or more embodiments or examples in a combined manner.

[0037] The embodiment of the present application discloses a kind of adsorbent dynamic adsorption detection method and equipment thereof.

[0038] As Figure 1 As shown in the flowchart of the adsorbent dynamic adsorption detection method provided by the embodiment of the present application, it includes the following steps: S100: the adsorbent is regenerated and treated to obtain regenerated adsorbent; S200: the temperature of the constant-temperature water bath is adjusted according to the required test temperature; S300: a specified weight of regenerated adsorbent is weighed and placed in the adsorption device and closed; S500: start the air compressor to output the gas source, adjust the pressure and flow to the test range, and make the gas source continuously transport the constant-temperature gas source to the adsorption device after passing through the constant-temperature water bath; S500: observe the dew point of the adsorption device, and close the air compressor when the dew point reaches the set threshold to stop the gas source; S600: open the adsorption device after the air compressor pressure drops to 0 Mpa, take out the adsorbed adsorbent and weigh its weight after adsorption to obtain the adsorption amount of the adsorbent, and judge the adsorption performance of the adsorbent according to the adsorption amount.

[0039] Among them, the regeneration treatment of the adsorbent means that the adsorbed gas of the adsorbent is removed to restore it to the original state before adsorption as much as possible, which is a pretreatment before detecting the adsorbent. The step of regeneration treatment specifically includes: Place the first container on the weighing platform to zero, take a sufficient amount of adsorbent into the first container according to the detection requirement, and place the first container and the adsorbent into the vacuum drying box for heating and drying; After reaching the set heating time, turn off the vacuum drying oven and open the exhaust valve to release pressure. After the pressure is released, remove the first container and the adsorbent and quickly place them in a dry dish and seal to cool. After cooling, the regenerated adsorbent is obtained.

[0040] The first container can be a 300ml beaker. Place the beaker on the weighing platform of a high-precision electronic balance and tare to zero. The precision of the electronic balance can be 0.1g. Then, place a sufficient amount of adsorbent into the beaker. The amount placed should ensure that the regenerated adsorbent meets the detection requirements. For example, 300g of adsorbent can be placed to ensure that the regenerated adsorbent is not less than 200g, which can be used for detection. After the amount is taken, place the beaker and the adsorbent in the beaker into the vacuum drying oven to heat and dry the adsorbent to evaporate the adsorbed gas and dry it. The heating temperature can be set to 250°C. The set heating time can be 6 hours. After 6 hours, turn off the vacuum drying oven and open its exhaust valve to release pressure. Wait until the negative pressure gauge returns to zero, indicating that the pressure release is complete. After a period of time, remove the beaker and quickly place it in a dry dish and seal it to prevent the adsorbent in the beaker from adsorbing air. Cool the beaker and adsorbent to room temperature. During cooling, you can use a timer to record the actual cooling time. The cooled adsorbent is the regenerated adsorbent.

[0041] After obtaining the regenerated adsorbent, prepare to test its adsorption capacity. Before testing, adjust the temperature of the constant temperature water bath according to the required test temperature to ensure that the test gas source reaches the required test temperature. The specific steps include: Make sure the water level of the constant temperature water bath is above the internal heat exchange tube. Set the temperature of the constant temperature water bath according to the ambient temperature. Adjust the water bath temperature so that the actual temperature of the water bath and the set temperature have a temperature difference within the set threshold range.

[0042] The heat exchange pipe is a pipeline for the gas source to flow. The gas source is output by an air compressor. The gas source enters the inside of the heat exchange pipe and exchanges heat with the constant temperature water bath to meet the experimental requirements of the gas source provided to the adsorption device. The constant temperature water bath is provided with heating devices and refrigeration devices, which can heat and cool the water bath to adjust the temperature of the water bath, and the actual temperature of the water bath is monitored in real time by a temperature controller. The required experimental temperature can be set differently according to the test environment, for example, when the ambient temperature is higher than 28℃, the constant temperature water bath is set to 25℃, when the ambient temperature is lower than 25℃, the constant temperature water bath is set to 25℃, when the ambient temperature is lower than 22℃, the constant temperature water bath is set to 26℃, and when the ambient temperature is lower than 16℃, the constant temperature water bath is set to 27℃. Thus, the inlet temperature of the adsorbent for testing is between 25-26℃. The temperature of the constant temperature water bath can also be set according to the working conditions of the adsorbent, for example, it can be applied to low temperature harsh working conditions, and the temperature of the constant temperature water bath can also be set to a low temperature accordingly. After setting the temperature of the constant temperature water bath, wait for a certain time, for example, 30 minutes, observe the actual temperature of the constant temperature water bath and the set temperature through the temperature controller, if the temperature difference between the two is not more than the set threshold range, for example, ±0.3℃, it is considered to meet the experimental requirements, and the heating or cooling can be stopped.

[0043] When the temperature of the constant temperature water bath meets the experimental requirements, the specified weight of the regenerated adsorbent needs to be weighed and placed in the adsorption device and closed, including the steps of: Record the temperature and humidity of the experimental environment and the actual time; Turn on the recorder and flow meter of the adsorption device, and in the case that the recorder time is consistent with the actual time, open the feed inlet and cover the funnel; Weigh the specified weight of the regenerated adsorbent, and pour the regenerated adsorbent into the adsorption device through the funnel; Cover the feed inlet and close it.

[0044] Record the temperature and humidity of the experimental environment as experimental data of different working conditions, which is convenient for subsequent data analysis. By confirming that the time displayed by the recorder is the same as the actual time, the experimental data is prevented from being chaotic and mismatched. The recorder is provided with a digital display panel, which can display real-time data of various parameters in the adsorption device, such as pressure, dew point, temperature, etc. The specified weight of the adsorbent is determined according to the experimental requirements and conditions, for example, 200g, and then introduced into the adsorption column through the funnel. The funnel is an accessory attached to the adsorption device, which is used to guide the adsorbent into the inside of the adsorption device, so as to avoid that the adsorbent flows to the outside due to the small size of the feed inlet. After the specified weight of the adsorbent enters the adsorption device, the funnel is removed, the feed inlet is covered and closed.

[0045] After the regenerated adsorbent enters the adsorption device, the air supply pipeline of the air compressor is connected with the inlet end of the heat exchange pipe of the constant temperature water bath, the air inlet pipeline of the adsorption device is connected with the outlet end of the heat exchange pipe of the constant temperature water bath, the air compressor is started, the air source first enters the constant temperature water bath for heat exchange treatment, and then is transported into the adsorption device, so that the adsorber in the interior adsorbs air, at the same time, the pressure is adjusted to a test range through the pressure relief valve, for example, the pressure should not exceed 8 bar, so as to prevent the air compressor from jumping, the flow is adjusted to a test range through the throttle valve, and real-time monitoring is carried out during the test to make fine adjustment, so as to ensure that the pressure value and the flow value are in the test range. The value of the dew point is observed through the digital display panel of the recorder, when the value of the dew point reaches a set threshold value, the adsorption is considered to be completed, and the air compressor is turned off.

[0046] After the adsorption is completed, the adsorbed adsorbent needs to be taken out and weighed, and the specific steps include: The second container is weighed and zeroed, the adsorption device is opened, the internal adsorbent is poured into the second container, the weight of the adsorbed adsorbent is weighed, and the volume of the second container is greater than that of the first container.

[0047] The second container can be an 800ml beaker, the beaker is placed on the electronic scale and zeroed, and the range of the electronic scale can be 2000g. The pressure value on the digital display panel is observed, after the pressure value is reduced to 0Mpa, a period of time, for example, 2 minutes, the adsorption device is opened, the internal adsorbent is poured into the second container, the weight after adsorption is weighed and recorded, the weight after adsorption is subtracted from the specified weight of the regenerated adsorbent poured into the adsorption device, the adsorption amount of the adsorbent is obtained, and the adsorption performance is judged according to the adsorption amount.

[0048] The application also provides an adsorbent adsorption detection equipment.

[0049] Embodiment one: please refer to Figure 2 , which is a schematic diagram of the adsorbent adsorption detection equipment provided by the embodiment one of the application. As shown in Figure 2 , it comprises a regeneration device 1, an air compressor 2, a constant temperature water bath device 3 and an adsorption device 4. The regeneration device 1 comprises a vacuum dryer (not shown in the figure), which is used for heating and drying regeneration treatment of the adsorbent, so as to make it recover to the original state as much as possible. The air compressor 2 is connected with and communicates with the air inlet end of the internal heat exchange pipe 32 of the constant temperature water bath device 3, so that the air source transported by the air compressor 2 is subjected to cold and hot exchange with the temperature of the water bath through the heat exchange pipe 32, to ensure that the temperature of the air source meets the test requirements. The air outlet end of the heat exchange pipe 32 is connected with and communicates with the adsorption device 4, so that the air source can enter the interior of the adsorption device 4.

[0050] As Figure 3The constant temperature water bath device 3 includes a water bath box 31 and a heat exchange pipe 32. The water level in the water bath box 31 is higher than the top of the heat exchange pipe 32, so as to cover the heat exchange pipe 32. The water bath box 31 is provided with an inlet 33 and an outlet 34 for the heat exchange pipe 32 to enter and exit. The inlet 33 and the outlet 34 are arranged above the heat exchange pipe 32 and above the water level, so as to avoid liquid leakage. The heat exchange pipe 32 is connected with the gas source pipeline through the pipeline joint by penetrating the inlet 33 and the outlet 34. The heat exchange pipe 32 can be made of copper pipe or aluminum pipe. In the embodiment, the heat exchange pipe 32 is arranged in a spiral shape, and the pitch is the same as the pipe diameter, that is, the adjacent spiral pipes are in contact with each other, so as to increase the total length of the heat exchange pipe 32, and the gas source is fully heat exchanged inside. The water bath box 31 is provided with a heating device (not shown in the figure) and a cooling device (not shown in the figure), so as to heat and cool the water bath to adjust the temperature. The water bath box 31 is also provided with a temperature sensor (not shown in the figure), which is connected with an external temperature controller (not shown in the figure).

[0051] Please refer to Figure 4 , which is a schematic view of the adsorption device provided in the embodiment. The adsorption device 4 includes an adsorption column 41, a quick end cover 42, a mounting frame 43, a flow meter 44, a recorder (not shown in the figure), a gas-water separation filter 46, a dew point detector 47, and a pressure sensor 48. The adsorption column 41 is clamped with the mounting frame 43. The adsorption column 41 is hollow inside, for containing adsorbent. The quick end cover 42 has two, which are connected with the bottom end and the top end of the adsorption column 41 respectively. The quick end cover 42 is provided with a gas pipe interface 421, for connecting with the gas source pipeline. The adsorption column 41 is provided with a wire mesh (not shown in the figure) at a position close to the bottom inside. The wire mesh is above the bottom gas pipe interface 421. The wire mesh is used to support the adsorbent when the adsorbent is poured, so as to prevent the adsorbent from directly sinking to the bottom. The quick end cover 42 is also connected with a temperature sensor 422, for sensing the temperature inside the adsorption column. The temperature sensor 422, the flow meter 44, the dew point detector 47, and the pressure sensor 48 are all connected with the recorder, so as to send data to the recorder for recording. The recorder includes a digital display panel 45, for displaying the temperature, pressure, dew point, and other data information inside the adsorption column 41. The adsorption device 4 also includes a hopper (not shown in the figure), which can be inserted into the adsorption column 41, for facilitating the pouring of the adsorbent.

[0052] As Figure 5 shown, the output gas source of the air compressor enters the gas-water separation filter 46 from the A pipeline after passing through the heat exchange pipe 32, and then passes through the gas pipe interface 421 at the bottom end of the adsorption column 41, the gas pipe interface 421 at the top end of the adsorption column 41, and the flow meter 44. Then, part of the gas source is discharged from the B pipeline, and part of the gas source is transported to the dew point detector 47 and then discharged from the C pipeline. Figure 5 The dashed part in the figure is the gas source pipeline.

[0053] When the adsorbent dynamic adsorption detection equipment provided in the embodiment of the application is used for detection, the working steps are as follows: Place the first container on the electronic scale weighing platform to zero. Pour the adsorbent to be detected into the first container. Put the first container and the adsorbent into the vacuum drying box of the regeneration device and close the box door, open the vacuum valve, close the exhaust valve, ensure that the oil in the vacuum pump meets the use requirements, plug in the power supply of the vacuum pump, and observe whether the negative pressure gauge reaches below-0.1 Mpa after a few minutes. If not, the pipeline and the vacuum pump need to be detected. Turn on the power supply of the vacuum drying box, set the heating temperature to 250 DEG C, and reset the timer to start timing. After regeneration, wait for the negative pressure gauge to return to zero and wait for a few minutes, then take out the first container from the vacuum drying box, quickly put it into the drying dish, tighten the cover, and cool it to room temperature. Check the water level of the constant temperature water bath device to ensure that the water level is higher than the heat exchange pipe, set the temperature of the water bath according to the laboratory environment, and heat or cool to adjust the temperature of the water bath until the set value and the actual value of the constant temperature water bath differ by not more than 0.3 DEG C. Record the actual experimental conditions, including but not limited to temperature, humidity, actual time, start the recorder of the adsorption device and the flowmeter, and confirm that the time of the recorder is consistent with the actual time. Connect the bottom end of the adsorption column with the quick end cap, connect the quick end cap with the gas source pipeline, and insert the funnel into the top end of the adsorption column. Place another first container on the electronic scale to zero, take out the regenerated adsorbent in the drying dish, pour 200g into the first container, quickly pour the 200g regenerated adsorbent into the adsorption column through the funnel, then connect the top end of the adsorption column with the quick end cap, connect the quick end cap with the gas source pipeline, and confirm whether the digital display panel of the recorder normally displays data. Start the air compressor and adjust the pressure of the pressure relief valve to 6.8-6.9 bar, adjust the throttle valve, adjust the flow to 50±1 LPM, and the gas source enters the heat exchange pipe of the constant temperature water bath device and continuously transports into the adsorption column. Observe the dew point of the digital display panel. When the dew point rises to-20 DEG C, turn off the air compressor. Place the second container on the electronic scale with a range of 2000g to zero, when the number panel pressure value is 0 Mpa, open the quick end cap of the adsorption column, pour the adsorbent in the adsorption column into the second container, weigh and record the actual weight, and judge the adsorption performance of the adsorbent according to the adsorption capacity of the adsorbent.

[0054] Taking the actual weight after adsorption as 236g as an example, the difference is obtained by subtracting the weight before adsorption 200g, and then the percentage value of the difference and the weight before adsorption is obtained. According to the relevant industry standard, whether the percentage value is within the specified range is determined, and then it is considered that the adsorption performance is qualified.

[0055] Embodiment two: please refer to Figures 6 to 11 , is a schematic view of the adsorption column and the quick end cover provided by the embodiment two of the application. The main difference between embodiment two and embodiment one is that the structures of the adsorption column and the quick end cover are different.

[0056] As Figure 6 shown, the adsorption device 4 includes an adsorption column 51 and a quick end cover 52, the adsorption column 51 is used to contain an adsorbent, and the quick end cover 52 is connected with the adsorption column 51 to seal the adsorption column 51. The quick end cover 52 has two, which are respectively connected with the top and bottom ends of the adsorption column 51, the adsorption column 51 includes a plurality of quick insertion slots 511 which are uniformly distributed in the circumferential direction, and the quick end cover 52 is provided with a plurality of insertion blocks 521 which are uniformly distributed in the circumferential direction, and the quick insertion slot 511 is matched with the insertion block 521; the quick insertion slot 511 includes a first slot section 5111 and a second slot section 5112, the first slot section 5111 is vertically arranged and the top end penetrates, the second slot section 5112 is arranged in the circumferential direction, one end of the second slot section 5112 is in communication with the bottom end of the first slot section 5111, and the other end is closed and inclined away from the first slot section, when the quick end cover 52 is connected with the adsorption column 51, the insertion block 521 is inserted from the top of the first slot section 5111, and then slides downward along the first slot section 5111 until the bottom of the first slot section 5111, and then the quick end cover 52 is rotated to move in the direction of the second slot section 5112, as the quick end cover 52 slides along the inclined second slot section 5112, the connection between the quick end cover 52 and the adsorption column 51 becomes tighter and tighter, thereby realizing the quick insertion of the quick end cover 52 and the adsorption column 51, and the second slot section 5112 is arranged in the circumferential direction, which can prevent the upward displacement of the quick end cover 52. By arranging the quick insertion slot 511 and the insertion block 521, the quick connection of the quick end cover 52 and the adsorption column 51 is realized, and the detection efficiency and convenience are improved.

[0057] The embodiment of the application is to Figure 6The shown direction is the up-down direction of the adsorption column 51, when the adsorbent is poured into the adsorption column 51, the bottom of the adsorption column 51 is first inserted and fixed with the quick end cover 52, and then the adsorbent is poured from the feed port at the top of the adsorption column 51, if necessary, a funnel (not shown in the figure) is first inserted into the feed port at the top of the adsorption column 51, and then the adsorbent is poured through the funnel. If the diameter of the quick end cover is smaller than the inner diameter of the adsorption column, it is inserted into the adsorption column, and the adsorbent may be squeezed into the gap between the two. The inner diameter of the quick end cover 52 in the second embodiment of the application is designed to be larger than the outer diameter of the adsorption column 51, so that the quick end cover 52 is sleeved on the outside of the adsorption column 51, and after connection, the top of the adsorption column 51 is in contact with the inner top surface of the quick end cover 52, which can prevent the adsorbent from being embedded between the gap of the quick end cover 52 and the adsorption column 51.

[0058] In this embodiment, the plug 521 is in a cylindrical shape, is arranged on the inner circumferential surface of the quick end cover 52, and is close to the bottom of the quick end cover 52. The width of the first groove section 5111 is greater than the diameter of the plug 521, so that the plug 521 can smoothly enter the first groove section 5111. The width of the second groove section 5112 is equal to or slightly greater than the diameter of the plug 521, so that the quick end cover 52 and the adsorption column 51 are tightly connected.

[0059] As shown in Figure 6 , the adsorption device 4 includes a sealing member 53, the quick end cover 52 is provided with a sealing groove 522, and the sealing member 53 is installed in the sealing groove 522. After the quick end cover 52 is connected with the adsorption column 51, it is sealed by the sealing member 53 to prevent gas leakage.

[0060] As shown in Figure 6 , a threaded interface 523 is provided at the center position of the quick end cover 52, which is used for connecting with an air inlet connector or an air outlet connector. The air inlet connector is connected with the air source pipeline of the air inlet, the air source pipeline of the air inlet is connected with the air outlet end of the heat exchange pipe 32, and the air outlet connector is connected with the air outlet pipeline. The threaded interface 523 of the quick end cover 52 at the bottom of the adsorption column 51 is connected with the air inlet connector, and the threaded interface 523 of the quick end cover 52 at the top of the adsorption column 51 is connected with the air outlet connector. A circular wire mesh is coaxially installed in the quick end cover 52 at the bottom, which is located above the threaded interface 523 to prevent the adsorbent from leaking out through the threaded interface 523.

[0061] As shown in Figure 6 , a plurality of vertical grooves 525 are arranged on the outer circumferential surface of the quick end cover 52, which facilitate technicians to grasp the quick end cover 52 and prevent hands from slipping when the quick end cover 52 is rotated.

[0062] As shown in Figure 7 and Figure 8As shown, during the detection process, if the pressure in the adsorption column 51 is too high, it may cause the quick end cover 52 to move circumferentially, affecting the sealing effect. In order to prevent this situation and ensure the sealing stability of the entire detection process, the adsorption device 4 also includes three limiting structures 55, which are evenly distributed along the circumference of the adsorption column 51. The limiting structure 55 includes a first mounting code 551, a limiting member 553 and a second mounting code 552, wherein there are two first mounting codes 551, and the two first mounting codes 551 are connected to the quick end cover 52 and are arranged opposite to each other. The limiting member 553 is in the shape of a T-shaped round rod, and its transverse rod is coaxially connected to the two first mounting codes 551 and can rotate within the two first mounting codes 551. The second mounting code 552 is connected to the adsorption column 51 and is located below the quick end cover 52, and corresponds to the position between the two first mounting codes 551. When the vertical rod of the limiting member 553 rotates to the bottom, it is engaged with the second mounting code 552, thereby limiting the circumferential displacement of the quick end cover 52 and ensuring the stability and sealing of the connection between the quick end cover 52 and the adsorption column 51. After the test is completed, when the adsorbent needs to be poured out, the three stoppers 553 can be rotated upward to release the locking relationship between the quick end cover 52 and the adsorption column 51. The quick end cover 52 can then be screwed to separate it from the second groove section 5112 and slide upward from the first groove section 5111 to separate from the adsorption column 51. The provision of the stopper structure 55 can quickly lock the quick end cover 52 and the adsorption column 51, preventing the quick end cover 52 from circumferential displacement and allowing the locking relationship to be quickly released, thereby improving convenience.

[0063] Please refer to Figures 9 to 11 , the adsorption device 4 also includes a chamber regulating member, and the chamber regulating member includes a sub-cavity member 55 provided in the adsorption column 51, and the sub-cavity member 55 is used to divide the internal cavity of the adsorption column 51 into a plurality of unconnected small cavities, so that a plurality of different adsorbents or different quantities of the same adsorbent can be detected at the same time. As for the adsorbent dynamic adsorption detection method provided above, the entire detection process takes a long time. If different adsorbents are detected one by one, it takes even more time. In the second embodiment, the adsorption column 51 is divided into a plurality of unconnected cavities 551, and different adsorbents can be placed for simultaneous detection, or adsorbents of different quantities can be detected, provided that the detection conditions of these adsorbents are the same. Figure 9 As shown, in the second embodiment, the adsorption column 51 is divided into three cavities 551. The length direction of the three cavities 551 is consistent with the length direction of the adsorption column 51. This allows for simultaneous testing of three adsorbents, or simultaneous testing of three different quantities of the same adsorbent, thereby shortening the overall testing time or obtaining more dimensional test data for evaluation. In other embodiments, the adsorption column 51 can also be divided into two cavities 551, four cavities 551, or five cavities 551, etc.

[0064] like Figure 10As shown, the three cavities 551 are all communicated with the threaded interface 523 of the quick end cover 52, so as to be communicated with the gas inlet / outlet pipeline, and in other embodiments, the three cavities 551 can also be provided with independent threaded interfaces 523.

[0065] As shown, Figure 11 As shown, the adsorption device 4 further comprises a pouring cover plate 56, which is used to be clamped with the cavity dividing member 55 to shield the feeding ports of two cavities 551 when the adsorbent needs to be poured out after the adsorption detection is completed, so that the cavity 551 not shielded can be poured first, thereby realizing that various adsorbents can be poured out independently without affecting each other.

[0066] Embodiment three: please refer to Figure 12 and Figure 13 , are schematic diagrams of the adsorption column provided in embodiment three of the present application. Embodiment three provides an adsorption column 61, a top end cover (not shown in the figure) and a bottom end cover 62, which are different from the adsorption column provided in embodiment one or embodiment two in that: the cavity adjusting member comprises a sub-adsorption column 613 arranged inside the adsorption column 61, the top of the sub-adsorption column 613 is lower than the top of the adsorption column 61, a first adsorption cavity 611 and a second adsorption cavity 612 are formed inside the adsorption column 61, the top end of the first adsorption cavity 611 is communicated with the second adsorption cavity 612, the bottom end of the first adsorption cavity 611 is open to be communicated with the gas source, the bottom end of the second adsorption cavity 612 is connected with the first adsorption cavity 611 integrally, the first adsorption cavity 611 and the second adsorption cavity 612 form a primary and secondary cavity, during detection, the adsorbent is guided into the first adsorption cavity 611 through the funnel to perform adsorption detection, when the amount of adsorbent is small, only the first adsorption cavity 611 needs to be used, if the amount of adsorbent is large, the volume of the first adsorption cavity 611 cannot accommodate the adsorbent, then the adsorbent can flow into the second adsorption cavity 612 through the top end of the first adsorption cavity 611, thereby the situation of testing different amounts of adsorbent can be adapted. Or, when two different kinds of adsorbents need to be tested at the same time, one kind of adsorbent is put into the first adsorption cavity 611, and the other kind of adsorbent is put into the second adsorption cavity 612, thereby the situation of testing different kinds of adsorbents at the same time can be adapted, and the testing efficiency is improved. The bottom end cover 62 is connected with the bottom end of the adsorption column 61, a gas inlet 621 of the gas source is arranged at the center position thereof, a plurality of gas outlets 622 of the gas source are arranged at the circumference of the gas inlet 621 in a spaced manner, the gas inlet 621 is communicated with the first adsorption cavity 611, a corresponding passage is arranged at the bottom of the second adsorption cavity 612 to be communicated with the plurality of gas outlets 622, the top end cover has the same structure as the bottom end cover 62, but does not have the gas inlet and outlet. The gas source enters through the gas inlet 621, flows to the bottom of the second adsorption cavity 612 through the top of the first adsorption cavity 611, and is discharged, so that the adsorbents in the first adsorption cavity 611 and the second adsorption cavity 612 can all be adsorbed.

[0067] Embodiment four: please refer toFigure 14 is a schematic view of the adsorption column provided in Embodiment Four of the present application. Embodiment Four differs from Embodiment Two in that the chamber adjusting member is adjusting structure 72, the bottom of adsorption column 71 is provided with bottom plate 711, a threaded hole is formed in the center of bottom plate 711, adjusting structure 72 comprises adjusting plate 721, adjusting screw 722, sealing gasket 723 and nut 724, adjusting plate 721 is arranged inside adsorption column 71 and is connected with adjusting screw 722, adjusting screw 722 is adapted to the threaded hole on bottom plate 711, and the handle of adjusting screw 722 can be turned to move adjusting plate 721 up and down inside adsorption column 71, so that the volume inside adsorption column 71 can be changed to adapt to different amounts of adsorbent for testing. Sealing gasket 723 is located between bottom plate 711 and nut 724, after the position of adjusting plate 721 is determined, nut 724 is rotated to move sealing gasket 723 towards bottom plate 711 until they are pressed against each other, the position where adjusting screw 722 is connected with the threaded hole is sealed by sealing gasket 723 to prevent air leakage. Adjusting screw 722 is provided with air inlet channel 725 in the center, air inlet channel 725 penetrates adjusting screw 722 and adjusting plate 721, and the air source can enter adsorption column 71 through air inlet channel 725, so that adjusting screw 722 not only plays a role in adjusting the position but also plays a role as an air source pipeline, and air inlet channel 725 changes accordingly with the change of the position of adjusting plate 721, so that the area inside adsorption column 71 that is actually tested can directly and quickly obtain the air source, and air inlet channel 725 is provided with a threaded port at one end of the handle and can be connected with an air inlet connector. The quick end cover at the top of adsorption column 71 can adopt the same structure as that of Embodiment Two.

[0068] It is understood that, although each step in the flowchart of the accompanying drawings is shown in sequence according to the arrow, these steps are not necessarily executed in sequence according to the arrow. Unless otherwise specified herein, the execution of these steps is not strictly limited in sequence, and they can be executed in other sequences.

[0069] The above are preferred embodiments of the present application, and do not limit the protection scope of the present application, therefore: any equivalent changes made on the structure, shape, principle of the present application shall be covered within the protection scope of the present application.

Claims

1. A dynamic adsorption detection method for an adsorbent, characterized in that: Including steps: regenerating the adsorbent to obtain a regenerated adsorbent; Adjust the temperature of the constant temperature water bath according to the required test temperature; Weigh the specified weight of regenerated adsorbent, place it into the adsorption device and seal it; Start the air compressor to output the gas source, adjust the pressure and flow rate to the test range, and allow the gas source to continuously deliver the constant temperature gas source to the adsorption device after passing through the constant temperature water bath; Observe the dew point of the adsorption device, and shut down the air compressor and stop delivering the gas source when the dew point reaches a set threshold; After the pressure drops to 0 MPa, the adsorption device is opened, the adsorbed adsorbent is taken out and its weight after adsorption is weighed to obtain the adsorption amount of the adsorbent, and the adsorption performance of the adsorbent is judged according to the adsorption amount.

2. The adsorbent dynamic adsorption detection method according to claim 1, characterized in that: The step of regenerating the adsorbent comprises: Place the first container on a weighing platform, peel and set to zero, take a sufficient amount of adsorbent according to the test requirements and put it into the first container, and place the first container and the adsorbent in a vacuum drying oven for heating and drying; After the set heating time is reached, close the vacuum drying oven and open the exhaust valve to release the pressure; After the pressure relief is completed, the first container and the adsorbent are taken out and quickly placed in a drying dish, sealed and cooled. After cooling is completed, the regenerated adsorbent is obtained.

3. The adsorbent dynamic adsorption detection method according to claim 1, characterized in that: The step of adjusting the temperature of the constant temperature water bath according to the required test temperature includes: Confirm that the water level of the constant temperature water bath is above the internal heat exchange tube, set the constant temperature water bath temperature according to the ambient temperature, and adjust the water bath temperature so that the temperature difference between the actual temperature of the water bath and the set temperature is within the set threshold range.

4. The adsorbent dynamic adsorption detection method according to claim 1, characterized in that: The steps of weighing a specified weight of the regenerated adsorbent, placing it into the adsorption device, and locking and sealing it include: Record the temperature, humidity and actual time of the experimental environment; Turn on the recorder and flow meter of the adsorption device. When the recorder time is consistent with the actual time, open the feed port of the adsorption device and insert the funnel; Weighing a specified weight of the regenerated adsorbent and pouring the regenerated adsorbent into the adsorption device through the funnel; The feed port is covered and sealed.

5. The adsorbent dynamic adsorption detection method according to claim 2, characterized in that: The step of taking out the adsorbent after adsorption and weighing its weight after adsorption comprises: The second container is weighed and set to zero, the adsorption device is opened, and the adsorbent inside is placed in the second container, and the weight of the adsorbent after adsorption is weighed. The volume of the second container is greater than that of the first container.

6. An adsorbent dynamic adsorption detection device, using the adsorbent dynamic adsorption detection method according to any one of claims 1 to 5, characterized in that: The invention comprises a regeneration device (1), an air compressor (2), a constant temperature water bath device (3) and an adsorption device (4), wherein the regeneration device (1) comprises a vacuum dryer, the air compressor (2) is connected to a heat exchange pipe (32) inside the constant temperature water bath device (3), and the heat exchange pipe (32) is connected to the adsorption device (4).

7. The adsorbent dynamic adsorption detection device according to claim 6, characterized in that: The adsorption device (4) includes a recorder, an adsorption column (41), a quick end cover (42), a flow meter (44), an air-water separation filter (46), a dew point detector (47) and a pressure sensor (48). The recorder is used to record and display the temperature and dew point data inside the adsorption column (41) and the flow and pressure data of the gas source. The adsorption column (41) is used to accommodate the adsorbent. There are two quick end covers (42), which are detachably connected to the top and bottom of the adsorption column (41), respectively. The air-water separation filter (46) is respectively connected to the quick end cover (42) at the bottom of the adsorption column (41) and the pressure sensor (48). The flow meter (44) is connected to the quick end cover (42) at the top of the adsorption column (41). The dew point detector (47) is connected to the flow meter (44).

8. The adsorbent dynamic adsorption detection device according to claim 6, characterized in that: The adsorption device (4) comprises an adsorption column (51) and a quick end cover (52), wherein the adsorption column (51) comprises a plurality of quick slots (511) uniformly distributed along the circumference, and the quick end cover (52) is provided with a plurality of plug blocks (521) uniformly distributed along the circumference, wherein the quick slots (511) are adapted to the plug blocks (521); the quick slots (511) comprise a first slot section (5111) and a second slot section (5112), wherein the first slot section (5111) is vertically arranged and has a top end extending therethrough, and the second slot section (5112) extends circumferentially, with one end thereof communicating with the bottom end of the first slot section (5111) and the other end being closed and inclined in a direction away from the top end of the first slot section (5111).

9. The adsorbent dynamic adsorption detection device according to claim 8, characterized in that: The adsorption device (4) includes a plurality of limiting structures (55), and the plurality of limiting structures (55) are evenly distributed along the circumference of the adsorption column (51). The limiting structure (55) includes two first mounting codes (551), a limiting member (553) and a second mounting code (552). The two first mounting codes (551) are connected to the quick end cover (52), and the second mounting code (552) is connected to the adsorption column (51). The limiting member (553) is rotatably connected to the two first mounting codes (551), and the limiting member (553) is snap-fitted to the second mounting code (552).

10. The adsorbent dynamic adsorption detection device according to claim 8, characterized in that: The adsorption device (4) comprises a chamber adjustment member, the chamber adjustment member is connected to the interior of the adsorption column (51), and the chamber adjustment member is used to adjust the volume within the adsorption column (51) to test adsorbents of different quantities.

Images