Reaction tube cleaning device

Abstract

The utility model provides a reaction tube cleaning device, and belongs to the technical field of hydrogen energy storage device cleaning. The reaction tube cleaning device comprises: a heating tank for accommodating and heating a reaction tube; the brush is used for cleaning the inner wall of the reaction tube; the cleaning liquid storage tank is provided with a liquid inlet and a liquid outlet, and the liquid inlet and the liquid outlet are both communicated with the heating tank; the hydraulic machine is arranged between the liquid inlet and the reaction tube. According to the reaction tube cleaning device, the reaction tube is arranged in the heating tank, and the cleaning liquid pressurized by the hydraulic machine is conveyed into the heating tank through the cleaning liquid storage tank, so that the reaction tube can be cleaned by the cleaning liquid under a certain heating condition and certain pressure, and meanwhile, the inner wall of the reaction tube is cleaned by the brush, so that the reaction tube can be fully cleaned; and the device is suitable for small reaction tubes with various specifications in an organic liquid hydrogen storage system.

Description

Technical Field

[0001] This utility model relates to the field of hydrogen energy storage device cleaning technology, and in particular to a reaction tube cleaning device. Background Technology

[0002] Ethylcarbazole, as one of the organic liquid hydrogen carriers, exhibits stable performance and high safety after hydrogenation, and can be stored at ambient temperature and pressure, similar to petroleum. It boasts a high hydrogen storage density, theoretically reaching 5.6% / wt. During the research and testing phase, N-ethylcarbazole, used as a hydrogen carrier, underwent addition and dehydrogenation reactions in a catalyst-filled reaction tube. After repeated cyclic experiments, due to its high melting point, strong viscosity, and tendency to solidify at room temperature, N-ethylcarbazole frequently adhered to the inner cavity of the reaction tube. This led to a gradual reduction in the amount of catalyst loaded, decreasing the porosity of the inner cavity and easily causing blockages, ultimately damaging the reaction tube and affecting hydrogen storage performance and efficiency. Therefore, periodic cleaning of the reaction tube is necessary.

[0003] Currently available cleaning equipment is difficult to use on small reaction tubes of various sizes. Utility Model Content

[0004] This invention provides a reaction tube cleaning device to solve the problem that existing cleaning equipment cannot be matched with small reaction tubes of various specifications in organic liquid hydrogen storage systems.

[0005] This utility model provides a cleaning device for cleaning reaction tubes in an organic liquid hydrogen storage system, comprising:

[0006] A heating bath, used to hold and heat the reaction tubes;

[0007] A brush, used to clean the inner wall of the reaction tube;

[0008] The cleaning fluid storage tank has an inlet and an outlet, both of which are connected to the heating tank;

[0009] A hydraulic press is positioned between the liquid inlet and the reaction tube.

[0010] The beneficial effects of the above-mentioned technical solution adopted in this application are as follows: by placing the reaction tube in the heating tank and supplying the cleaning fluid pressurized by the hydraulic press into the heating tank from the cleaning fluid storage tank, the reaction tube can be cleaned by the cleaning fluid under certain heating conditions and pressure. At the same time, the inner wall of the reaction tube is cleaned by a brush, thereby achieving thorough cleaning of the reaction tube. This method is applicable to small reaction tubes of various specifications in organic liquid hydrogen storage systems.

[0011] Based on the above technical solution, the present invention can be further improved as follows:

[0012] Furthermore, the extension direction of the heating tank and the extension direction of the reaction tube are both vertical, and the liquid inlet and the liquid outlet are respectively connected to the two ends of the extension direction of the heating tank.

[0013] The beneficial effect of adopting the above technical solution in this utility model is that by setting the extension direction of the heating tank and the extension direction of the reaction tube to be vertical, the cleaning liquid can better contact the reaction tube and clean it.

[0014] Furthermore, an inlet valve is provided on the pipe between the liquid inlet and the heating tank, and an outlet valve is provided on the pipe between the liquid outlet and the heating tank.

[0015] Furthermore, the two ends of the heating tank in the extension direction are respectively connected to an air inlet pipe and an air outlet pipe, an air inlet valve is provided on the air inlet pipe, and an air outlet valve is provided on the air outlet pipe.

[0016] The beneficial effect of adopting the above technical solution in this application is that by setting up an inlet pipe and an outlet pipe, the reaction tube can be further purged with gas, thereby achieving better cleaning of the reaction tube.

[0017] Furthermore, the brush is connected to a motor, and the motor can drive the brush to rotate within the reaction tube; and / or

[0018] The surface of the heating tank is provided with heat-insulating components; and / or

[0019] The cleaning device also includes a bracket with a slot on it, and the heating tank is engaged in the slot.

[0020] The beneficial effects of adopting the above technical solution in this utility model are: by setting a motor, automatic cleaning of the reaction tube can be achieved; and by setting a heat-insulating component, the heating tank can be kept warm.

[0021] Furthermore, the cleaning device also includes a controller, which is communicatively connected to the heating tank, the liquid inlet valve, the liquid outlet valve, the air inlet valve, the air outlet valve, and the motor.

[0022] The beneficial effects of adopting the above technical solution in this utility model are: by setting a controller, the heating tank, liquid inlet valve, liquid outlet valve, air inlet valve, air outlet valve and motor can be controlled by the controller, thereby better controlling the reaction tube cleaning process. Attached Figure Description

[0023] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with the present invention and, together with the description, serve to explain the principles of the present invention.

[0024] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 A schematic diagram of the structure of a cleaning device for cleaning reaction tubes in an organic liquid hydrogen storage system provided in an embodiment of this application;

[0026] Figure 2 This is the chromatogram of S1 provided in Example 1 of this application;

[0027] Figure 3 This is the chromatogram of D1 provided in Comparative Example 1 of this application;

[0028] Among them, 1-insulation component; 2-heating tank; 3-reaction tube; 4-connecting rod; 5-brush; 6-inlet valve; 7-outlet valve; 8-slot; 9-controller; 10-bracket; 11-hydraulic press; 12-cleaning fluid storage tank; 13-motor; 14-air inlet valve; 15-air outlet valve. Detailed Implementation

[0029] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Experimental methods in the following embodiments that do not specify specific conditions are generally determined according to national standards. If there is no corresponding national standard, then general international standards, conventional conditions, or conditions recommended by the manufacturer shall be followed.

[0030] like Figure 1 As shown, this utility model provides a cleaning device for cleaning reaction tubes in an organic liquid hydrogen storage system, comprising:

[0031] Heating tank 2 is used to house and heat reaction tube 3;

[0032] Brush 5 is used to clean the inner wall of the reaction tube 3;

[0033] The cleaning fluid storage tank 12 has an inlet and an outlet, both of which are connected to the heating tank 2;

[0034] The hydraulic press 11 is located between the liquid inlet and the reaction tube 3.

[0035] Based on the above technical solution, the present invention can be further improved as follows:

[0036] Furthermore, the extension direction of the heating tank 2 and the extension direction of the reaction tube 3 are both vertical, and the liquid inlet and the liquid outlet are respectively connected to the two ends of the extension direction of the heating tank 2.

[0037] Furthermore, an inlet valve 6 is provided on the pipe between the liquid inlet and the heating tank 2, and an outlet valve 7 is provided on the pipe between the liquid outlet and the heating tank 2.

[0038] Furthermore, the two ends of the heating tank 2 in the extension direction are respectively connected to an air inlet pipe and an air outlet pipe, an air inlet valve 14 is provided on the air inlet pipe, and an air outlet valve 15 is provided on the air outlet pipe.

[0039] Furthermore, the brush 5 is connected to the motor 13, and the motor 13 can drive the brush 5 to rotate within the reaction tube 3; and / or

[0040] The surface of the heating tank 2 is provided with a heat insulation component 1; and / or

[0041] The cleaning device also includes a bracket 10, on which a slot 8 is provided, and the heating tank 2 is engaged in the slot 8.

[0042] Furthermore, the cleaning device also includes a controller 9, which is communicatively connected to the heating tank 2, the liquid inlet valve 6, the liquid outlet valve 7, the air inlet valve 14, the air outlet valve 15 and the motor 13. Example

[0043] This embodiment provides a reaction tube cleaning device, including the following steps:

[0044] (1) Assembly of cleaning device: The surface of the heating tank 2 is covered with a heat insulation component 1, which is a heat insulation plate. The bottom of the heating tank 2 is connected to the slot 8 on the bracket 10, thereby fixing the heating tank 2 on the bracket 10 and extending the heating tank 2 in the vertical direction. The outlet of the cleaning fluid storage tank 12, the hydraulic device 11, and the bottom of the heating tank 2 are connected in sequence through pipes. The top of the heating tank 2 is connected to the inlet of the cleaning fluid storage tank 12. At the same time, the bottom and top of the extension direction of the heating tank are also connected to air inlets. Install the inlet valve 6, outlet valve 7, inlet valve 14, and outlet valve 15 on the pipe between the inlet of the cleaning liquid storage tank 12 and the heating tank 2, the pipe between the outlet of the cleaning liquid storage tank 12 and the heating tank 2, the inlet pipe, and the outlet pipe, respectively. Place the reaction tube 3 to be cleaned into the heating tank 2, with the inlet and outlet of the reaction tube 3 set vertically. Place the brush 5 into the reaction tube 3 and connect it to the motor 13 through the connecting rod 4. Cover and tighten the cover to seal the reaction tube 3.

[0045] (2) First cleaning: Pour 300mL of ethylcyclohexane into the cleaning liquid storage tank 12, open the inlet valve 6 and the outlet valve 7, close the inlet valve 14 and the outlet valve 15, then set the hydraulic pressure of the hydraulic press 11 to 4MPa, the heating temperature of the heating tank 2 to 60℃, the heating time to 0.5h, and the rotation speed of the brush 5 to 500r / min, so that the ethylcyclohexane circulates in the liquid pipeline and cleans for 0.5h. After cleaning, close the outlet at the bottom of the cleaning liquid storage tank 12, wait for all the refluxed ethylcyclohexane to return to the cleaning liquid storage tank 12, then turn off the hydraulic press 11 and the brush 5, pour out the ethylcyclohexane in the cleaning liquid storage tank 12, and replace it with a new 300mL of ethylcyclohexane in the cleaning liquid storage tank 12.

[0046] (3) Second wash: Repeat the first wash process to perform a second wash, and then collect the ethylcyclohexane after the second wash;

[0047] (4) Purge: Open the inlet valve 6 and outlet valve 7, open the inlet valve 14 and outlet valve 5, and introduce nitrogen gas through the inlet pipe. The gas pressure is 0.1 MPa and the purging time is 0.5 h. At the same time, the heating temperature of the heating tank on the controller 9 is set to 150 °C and the rotation speed of the brush 5 is 500 r / min. After the purging is completed, close all circuits and valve switches. After the heater cools down to room temperature, take out the reaction tube to complete the cleaning. Example

[0048] This embodiment is basically the same as embodiment 1, except that in this embodiment, the hydraulic pressure is 6 MPa and the heating temperature is 80°C during the first and second cleaning processes. Example

[0049] This embodiment is basically the same as embodiment 1, except that in this embodiment, the hydraulic pressure is 8 MPa and the heating temperature is 100°C during the first and second cleaning processes. Example

[0050] This embodiment is basically the same as embodiment 1, except that in this embodiment, the hydraulic pressure is 4 MPa and the heating temperature is 120°C during the first and second cleaning processes.

[0051] Comparative Example 1:

[0052] This comparative example is basically the same as Example 1, except that ethylcyclohexane is replaced with anhydrous ethanol in this comparative example.

[0053] Comparative Example 2:

[0054] This comparative example is basically the same as Example 1, except that in this comparative example, the hydraulic pressure is 4 MPa during the first and second cleaning processes, and the heating function of the heating tank 2 is turned off.

[0055] Comparative Example 3:

[0056] This comparative example is basically the same as Example 1, except that in the first and second cleaning processes of this comparative example, the hydraulic pressure is 4 MPa and the heating temperature is 150°C.

[0057] Test example: Ethylcyclohexane after the second washing of the examples and comparative examples was collected and named S1, S2, S3, S4, D1, D2 and D3, respectively, and subjected to chromatographic analysis. The results are shown in Table 1.

[0058] Table 1. Comparison of material purity after different cleaning methods in the examples and comparative examples.

[0059]

[0060] As shown in Table 1, in Examples 1-4, using ethylcyclohexane as the cleaning fluid, with heating temperatures between 60℃ and 120℃ and hydraulic pressures between 4 and 8 MPa, the collected liquids after 1.0 h of cleaning all achieved a purity of over 99.0%. In contrast, Comparative Example 1, using anhydrous ethanol, had a purity of only about 83.31%, demonstrating a significantly improved cleaning effect. Comparative Example 2 had a purity of 98.47%, which was slightly lower, while Comparative Example 3 had a purity of 95.55%, a substantial decrease. Because anhydrous ethanol has a lower boiling point and lower solubility than ethylcyclohexane, it is less effective at cleaning. Within a suitable temperature range, the solubility of ethylcyclohexane is fully utilized, greatly enhancing the cleaning effect. However, excessively high temperatures cause ethylcyclohexane to evaporate, reducing the cleaning efficiency.

[0061] Table 2 shows the detection data of liquid S1 collected after two cleanings using ethylcyclohexane as the cleaning solution in Example 1 of this application, obtained by chromatograph analysis. Table 3 shows the detection data of liquid D1 collected after two cleanings using anhydrous ethanol as the cleaning solution in Comparative Example 1 of this application, obtained by chromatograph analysis.

[0062] Table 2

[0063] Table 3

[0064] In Tables 2 and 3, retention time refers to the time from injection to reaching the peak. Peak area is the elution area of ​​the substance, representing its relative content. Peak height indicates the peak height, and area percentage refers to the area ratio between peaks, also indicating the purity of each substance. In the S1 chromatogram of Table 2, the peak with the largest peak height is ethylcyclohexane. In the D1 chromatogram of Table 3, the peak with the largest peak height is anhydrous ethanol; the remaining peaks are residues. As can be seen from Tables 2 and 3, this application, by selecting ethylcyclohexane and cleaning the reaction tube at a suitable temperature, removes most of the residues, achieving a purity of over 99% within the tube.

[0065] The above description is merely a specific embodiment of the present invention, enabling those skilled in the art to understand or implement the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed herein.

Claims

1. A reaction tube cleaning device, characterized in that, include: A heating bath, used to hold and heat the reaction tubes; A brush, used to clean the inner wall of the reaction tube; The cleaning fluid storage tank has an inlet and an outlet, both of which are connected to the heating tank; A hydraulic press is positioned between the liquid inlet and the reaction tube.

2. The reaction tube cleaning device according to claim 1, characterized in that, The extension direction of the heating tank and the extension direction of the reaction tube are both vertical, and the liquid inlet and the liquid outlet are respectively connected to the two ends of the extension direction of the heating tank.

3. The reaction tube cleaning device according to claim 2, characterized in that, An inlet valve is installed on the pipe between the liquid inlet and the heating tank, and an outlet valve is installed on the pipe between the liquid outlet and the heating tank.

4. The reaction tube cleaning device according to claim 3, characterized in that, The heating tank is connected to an air inlet pipe and an air outlet pipe at both ends of its extension direction. An air inlet valve is provided on the air inlet pipe, and an air outlet valve is provided on the air outlet pipe.

5. The reaction tube cleaning device according to claim 4, characterized in that, The brush is connected to a motor, and the motor can drive the brush to rotate inside the reaction tube; and / or The surface of the heating tank is provided with heat-insulating components; and / or The cleaning device also includes a bracket with a slot, and the heating tank is engaged in the slot.

6. The reaction tube cleaning device according to claim 5, characterized in that, The cleaning device also includes a controller, which is communicatively connected to the heating tank, the liquid inlet valve, the liquid outlet valve, the air inlet valve, the air outlet valve, and the motor.

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