Coal hydro-liquefaction reaction device with gas-liquid interface oscillation and use method of coal hydro-liquefaction reaction device

Abstract

The invention discloses a gas-liquid interface oscillation coal hydrogenation liquefaction reaction device and a use method thereof. The device comprises a reaction kettle body, a stirring device, a swinging device and a control device, the stirring device is arranged in the reaction kettle body and is used for stirring materials in the reaction kettle body, and the swinging device is arranged outside the reaction kettle body, is connected with the outer wall surface of the reaction kettle body and is used for driving the reaction kettle body to swing at different frequencies and different angles so as to simulate gas-liquid interface oscillation in the reaction process; the stirring device and the swinging device are electrically connected with the control device respectively; the oscillation amplitude of the gas-liquid interface is controlled by changing the swing angle and the swing frequency of the reaction device, the problem of wall surface coking caused by oscillation of the gas-liquid interface can be researched under high-temperature and high-pressure conditions by adopting the device, and equipment support can be provided for optimization of direct coal liquefaction, coal tar hydrogenation and heavy oil hydrogenation technologies.

Description

Technical Field

[0001] The invention relates to the fields of chemical engineering and material engineering, and in particular to a coal hydrogenation liquefaction reaction device with gas-liquid interface oscillation and a use method thereof. Background Art

[0002] Coal direct liquefaction technology can transform solid coal into clean and efficient liquid fuel, which can alleviate the problem of oil resource shortage to a certain extent. During the long-term operation of coal direct liquefaction industrial equipment, it was found that the high viscosity of oil-coal slurry and high-temperature coking of preheaters and hydrogenation reactors directly affected the long-term stable operation of coal direct liquefaction reaction equipment, which in turn determined the technical level and economy of coal direct liquefaction. In the hydrogenation liquefaction reactor, due to the existence of gas-liquid-solid three-phase flow and the disturbance caused by the gas passing through the reactor, the oil-coal slurry interface constantly oscillates and washes the high-temperature reactor wall. Some asphaltene adhering to the reactor wall will intermittently detach from the liquid during the oscillation of the gas-liquid interface. This part of the asphaltene is prone to condensation and coking reaction due to the difficulty in effectively obtaining active hydrogen. In addition, there is also the problem of wall coking caused by gas-liquid interface oscillation during coal tar hydrogenation and heavy oil hydrogenation.

[0003] At present, the high-pressure reactor for direct coal liquefaction can only meet the basic needs of laboratory research on direct coal liquefaction. There is no gas-liquid interface oscillation reaction device under high temperature and high pressure conditions, resulting in few research reports on the wall coking phenomenon caused by gas-liquid interface oscillation, which affects the research progress of the wall coking problem caused by gas-liquid interface oscillation. Summary of the invention

[0004] In view of the problems existing in the prior art, the present invention provides a coal hydroliquefaction reaction device with gas-liquid interface oscillation and a method of using the same, which provides equipment support for studying the wall coking problem caused by gas-liquid interface oscillation under high temperature and high pressure conditions.

[0005] The technical solution of the present invention is as follows:

[0006] In a first aspect of the present invention, there is provided a coal hydroliquefaction reaction device with gas-liquid interface oscillation, comprising a reaction kettle body, a stirring device, a swinging device and a control device;

[0007] The stirring device is arranged inside the reactor body and is used to stir the materials inside the reactor body. The swing device is arranged outside the reactor body and is connected to the outer wall of the reactor body and is used to drive the reactor body to swing at different frequencies and angles to simulate the oscillation of the gas-liquid interface during the reaction process.

[0008] The stirring device and the swinging device are electrically connected to the control device respectively.

[0009] In some embodiments of the present invention, a reactor cover is disposed on the top of the reactor body, the reactor cover is sealedly connected to the reactor body, and a gas inlet is disposed on the reactor cover.

[0010] In some embodiments of the present invention, the stirring device includes a first drive motor and a stirring paddle, and the output shaft of the first drive motor is fixedly connected to the stirring paddle.

[0011] In some embodiments of the present invention, the first drive motor is installed on the reactor cover, and the stirring paddle is located in the reactor body and close to the bottom of the reactor body.

[0012] In some embodiments of the present invention, the swing device includes a second drive motor, a connecting rod and a limit device, the output shaft of the second drive motor is fixedly connected to the reactor body through the connecting rod, and the limit device is arranged on the connecting rod between the reactor body and the second drive motor.

[0013] In some embodiments of the present invention, the limiting device includes a metal rod and an arc-shaped magnetic induction device, one end of the metal rod is vertically connected to the connecting rod, and the other end of the metal rod is placed in the arc-shaped magnetic induction device. The limiting device is used to control the reaction kettle body to swing at different angles.

[0014] In some embodiments of the present invention, a thermocouple is provided in the reactor body, and the thermocouple is electrically connected to a control device.

[0015] In a second aspect of the present invention, a method for using a coal hydroliquefaction reaction device with gas-liquid interface oscillation is provided, comprising the following steps:

[0016] Add materials into the reactor body, seal the reactor body, fill a certain amount of gas into the reactor body, maintain the required initial pressure, and then set the temperature rise program through the control device to control the reaction time and reaction temperature;

[0017] Turn on the stirring device and the swing device, fully stir the materials through the stirring device, and drive the reaction kettle to swing through the swing device;

[0018] The above device is maintained in operation for a required time. After the reaction is completed, the reactor body is cooled and depressurized, and the wall coking position caused by the oscillation of the gas-liquid interface in the reactor is sampled.

[0019] In some embodiments of the present invention, the control device controls the swing frequency by controlling the swing device and controls the swing angle by controlling the limit device to simulate the different contact surfaces between the gas-liquid interface and the inner wall of the reactor body during the reaction process.

[0020] In some embodiments of the present invention, the required gas is charged through the gas inlet on the reactor cover, the reading on the pressure gauge is observed to determine the initial pressure of the reaction, and the pressure changes during the reaction and at the end of the reaction are observed through the pressure gauge.

[0021] One or more technical solutions of the present invention have the following beneficial effects:

[0022] The coal hydroliquefaction reaction device with gas-liquid interface oscillation of the present invention is used to study the wall coking phenomenon caused by gas-liquid interface oscillation under high temperature and high pressure conditions. The gas-liquid interface fluctuation in the reactor is realized by the arranged swing device, which provides the possibility of obtaining the operation of the industrial device under real conditions. The operating temperature and pressure range of the device is wide and can be used for the study of the hydrocoking properties of different raw materials. The swing device can be adjusted in multiple directions and the frequency is controllable, which can control the conditions of different contact surfaces between solid and liquid during the reaction process. In addition, the device can also study the hydrocoking behavior of different raw materials to meet the needs of different scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of a coal hydroliquefaction reaction device with gas-liquid interface oscillation according to the present invention;

[0024] Figure 2 It is a schematic diagram of the swing of the reaction kettle body of the present invention;

[0025] Figure 3 Schematic diagram of the limiting device of the present invention.

[0026] In the figure: 1. reactor body; 2. reactor cover; 3. thermocouple; 4. control device; 5. first drive motor; 6. connecting rod; 7. limit device; 8. second drive motor; 9. stirring paddle; 10. output shaft; 11. stirring device; 12. swing device; 13. metal connecting rod; 14. magnetic induction device. DETAILED DESCRIPTION

[0027] The present invention will be further described below in conjunction with the accompanying drawings and embodiments.

[0028] Example 1

[0029] In a typical embodiment of the present invention, a coal hydroliquefaction reaction device with gas-liquid interface oscillation is provided, such as Figure 1 As shown, it includes a reaction kettle body 1, a stirring device 11, a swing device 12 and a control device 4;

[0030] The stirring device 11 is arranged in the reactor body 1, and is used to stir the materials in the reactor body 1. The swinging device 12 is arranged outside the reactor body 1 and connected to the outer wall surface of the reactor body 1, and is used to drive the reactor body 1 to swing at different frequencies and angles to simulate the oscillation of the gas-liquid interface during the reaction process.

[0031] The stirring device 11 and the swinging device 12 are electrically connected to the control device 4 respectively.

[0032] Furthermore, a reactor cover 2 is provided on the top of the reactor body 1, and the reactor cover 2 is sealed to the reactor body 1 to provide a high-temperature and high-pressure sealed environment for the reaction process. The reactor body 1 can withstand a reaction temperature from room temperature to 480°C and a pressure from normal pressure to 20MPa. A gas inlet is provided on the reactor cover for filling gas into the reactor body 1 for pressurization.

[0033] In this embodiment, the stirring device 11 includes a first drive motor 5 and a stirring paddle 9. The output shaft 10 of the first drive motor 5 is fixedly connected to the stirring paddle 9. The first drive motor 5 drives the stirring paddle to rotate via the output shaft 10 to achieve stirring of the material in the reactor body 1.

[0034] Furthermore, the first driving motor 5 is installed on the reactor cover 2, and the stirring paddle 9 is located in the reactor body 1 and close to the bottom of the reactor body.

[0035] In this embodiment, the swing device 12 includes a second drive motor 8 , a connecting rod 9 and a limiting device 7 . The output shaft of the second drive motor 8 is fixedly connected to the reactor body 1 through the connecting rod 9 , and the limiting device 7 is arranged on the connecting rod 6 .

[0036] Furthermore, the limit device includes a metal rod 13 and a magnetic induction device 14, one end of the metal rod 13 is vertically connected to the connecting rod 6, and the other end of the metal rod 13 is placed in the arc-shaped magnetic induction device 14, and the limit device is used to control the reaction kettle body to swing at different angles. The magnetic induction device adopts an existing structure, and the magnetic induction device controls the metal rod 13 to swing in the arc-shaped magnetic induction device 14 through a magnetic induction program, thereby controlling the swing amplitude of the reaction kettle body.

[0037] The swing device 12 can swing the reactor body 1 in multiple directions as required by adjusting the position of the connecting rod. At this time, the connecting rod is detachably fixedly connected to the reactor body 1.

[0038] In this embodiment, a thermocouple 3 is provided in the reactor body 1, and the thermocouple 3 is electrically connected to the control device 4. The temperature in the reactor body 1 is collected in real time through the thermocouple 3 and transmitted to the control device 4 for display. At the same time, the control device 4 controls the temperature in the reactor according to the temperature required for the reaction. Further, the control device 4 also controls the stirring rate and stirring time of the stirring device 11 and the swing rate of the swing device 12 to ensure the precise control of various parameters, further improving the accuracy and reliability of the experiment.

[0039] The method of using the coal hydroliquefaction reaction device with gas-liquid interface oscillation provided in this embodiment is as follows:

[0040] Before the liquefaction coking reaction is carried out, the reactor cover 2 is first opened, and then the materials are poured into the reactor body 1, the reactor body 1 is sealed by the reactor cover 2, and the required gas is filled in to maintain the required initial pressure, and then the temperature rise program is set by the control device 4 to control the reaction time and reaction temperature;

[0041] The stirring device 11 and the swinging device 12 are turned on, and the control device 4 is used to control the reactor body to swing at an angle of 0° to 50° and a swing frequency of 2 to 50s / time. The reactor body 1 is connected to the reactor body 1 through the connecting rod 6 to control the reactor body 1 to swing at a desired posture frequency, and the swinging can be performed in different directions; the control device 4 controls the second drive motor 8 to rotate, thereby driving the output shaft 10 and the stirring paddle 9 to rotate about the center of the circle to fully stir the material. The stirring rate can be adjusted according to the reaction requirements to ensure that the material is evenly mixed during the reaction process, thereby accelerating the reaction and improving production efficiency.

[0042] When the material reaches the target reaction temperature, this temperature is maintained, and the reaction is set for the required time, while maintaining the operation of the swing device 12 and the stirring device 11; after the set time is over, it enters the cooling stage, and when it is cooled to room temperature, the swing device 12 and the stirring device 11 are stopped, and the kettle cover 2 is opened after the pressure is released for sampling.

[0043] Example 2

[0044] In a typical embodiment of the present invention, a method for using a coal hydroliquefaction reaction device with gas-liquid interface oscillation is provided, comprising the following steps:

[0045] Add materials into the reactor body, seal the reactor body, fill a certain amount of gas into the reactor body, maintain the required initial pressure, and then set the temperature rise program through the control device to control the reaction time and reaction temperature;

[0046] Turn on the stirring device and the swing device, fully stir the materials through the stirring device, and drive the reaction kettle to swing through the swing device;

[0047] The above device is maintained in operation for a required time. After the reaction is completed, the reactor body is cooled and depressurized, and the wall coking position caused by the oscillation of the gas-liquid interface in the reactor is sampled.

[0048] Furthermore, the control device controls the swing angle and the swing frequency of the swing device to simulate the different contact surfaces between the gas-liquid interface and the inner wall of the reactor body during the reaction process.

[0049] By changing the swing angle and swing frequency of the reaction device to control the amplitude of the gas-liquid interface oscillation, the wall coking problem caused by the gas-liquid interface oscillation can be studied under high temperature and high pressure conditions, which can provide equipment support for the optimization of direct coal liquefaction, coal tar hydrogenation and heavy oil hydrogenation technology.

[0050] Furthermore, the required gas is charged through the gas inlet on the reactor cover, the reading on the pressure gauge is observed to determine the initial pressure of the reaction, and the pressure conditions during the reaction and at the end of the reaction are observed through the pressure gauge.

[0051] Although the above describes the specific implementation mode of the present invention in conjunction with the accompanying drawings, it is not intended to limit the scope of protection of the present invention. Those skilled in the art should understand that various modifications or variations that can be made by those skilled in the art on the basis of the technical solution of the present invention without creative work are still within the scope of protection of the present invention.

Claims

1. A coal hydroliquefaction reaction device with gas-liquid interface oscillation, characterized in that: It includes a reaction kettle body, a stirring device, a swinging device and a control device; The stirring device is arranged inside the reactor body and is used to stir the materials inside the reactor body. The swing device is arranged outside the reactor body and is connected to the outer wall of the reactor body and is used to drive the reactor body to swing at different frequencies and angles to simulate the oscillation of the gas-liquid interface during the reaction process. The stirring device and the swinging device are electrically connected to the control device respectively.

2. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 1, characterized in that: A reactor cover is arranged on the top of the reactor body, the reactor cover is sealed and connected to the reactor body, and a gas inlet is arranged on the reactor cover.

3. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 2, characterized in that: The stirring device comprises a first driving motor and a stirring paddle, and the output shaft of the first driving motor is fixedly connected to the stirring paddle.

4. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 3, characterized in that: The first driving motor is installed on the reactor cover, and the stirring paddle is located in the reactor body and close to the bottom of the reactor body.

5. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 1, characterized in that: The swing device includes a second drive motor, a connecting rod and a limiting device. The output shaft of the second drive motor is fixedly connected to the reactor body through the connecting rod. The limiting device is arranged on the connecting rod between the reactor body and the second drive motor.

6. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 5, characterized in that: The limiting device comprises a metal rod and an arc-shaped magnetic induction device, one end of the metal rod is vertically connected to the connecting rod, and the other end of the metal rod is placed in the arc-shaped magnetic induction device. The limiting device is used to control the reaction kettle body to swing at different angles.

7. The coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 1, characterized in that: A thermocouple is arranged in the reactor body and is electrically connected to the control device.

8. A method for using the coal hydroliquefaction reaction device with gas-liquid interface oscillation according to any one of claims 1 to 7, characterized in that: The following steps are involved: Add materials into the reactor body, seal the reactor body, fill a certain amount of gas into the reactor body, maintain the required initial pressure, and then set the temperature rise program through the control device to control the reaction time and reaction temperature; Turn on the stirring device and the swing device, fully stir the materials through the stirring device, and drive the reaction kettle to swing through the swing device; The above device is maintained in operation for a required time. After the reaction is completed, the reactor body is cooled and depressurized, and the wall coking position caused by the oscillation of the gas-liquid interface in the reactor is sampled.

9. The method for using the coal hydroliquefaction reaction device with gas-liquid interface oscillation as claimed in claim 8, characterized in that: The control device controls the swing frequency by controlling the swing device, and controls the swing angle by controlling the limit device, so as to simulate the different contact surfaces between the gas-liquid interface and the inner wall of the reactor body during the reaction process.

10. The method for using the coal hydroliquefaction reaction device with gas-liquid interface oscillation according to claim 8, characterized in that: Fill the required gas through the gas inlet on the reactor cover, observe the reading on the pressure gauge to determine the initial pressure of the reaction, and observe the pressure changes during the reaction and at the end of the reaction through the pressure gauge.

Images