Fluidized bed device for chemical chain oxygen carrier performance test and test method thereof

Abstract

The invention relates to a fluidized bed device for testing the performance of a chemical chain oxygen carrier and a testing method thereof, and the fluidized bed device for testing the performance of the chemical chain oxygen carrier comprises a heating furnace which is internally provided with an oxygen carrier for testing, the oxygen carrier is arranged in a vertically arranged quartz tube, and the heating furnace heats the oxygen carrier to a fluidized state; a finished product outlet is formed in the upper end of the quartz tube; an outlet of the oxidizing gas cylinder is connected with the raw material inlet through a first pipeline; an outlet of the reducing gas cylinder is connected with the raw material inlet through a second pipeline; the oxidizing gas cylinder and the reducing gas cylinder are sequentially communicated with the raw material inlet, so that the oxygen carrier is sequentially and circularly subjected to oxidation-reduction reaction. According to the device, the oxidation-reduction reaction can be simultaneously carried out, the oxygen carrier does not need to be transferred, the oxidation-reduction reaction can be immediately carried out by switching the oxidizing gas and the reducing gas, the detection efficiency is high, and the labor intensity is low.

Description

Technical Field

[0001] The invention relates to the technical field of fluidized beds, in particular to a fluidized bed device for testing the performance of a chemical chain oxygen carrier and a testing method thereof. Background Art

[0002] Chemical looping process is a new type of process that decomposes an overall chemical reaction into multiple sub-reactions occurring in different reactors. It is widely used in energy and environmental engineering due to its characteristics of self-separation of products and no need for additional energy consumption, such as chemical looping combustion, chemical looping gasification and chemical looping reforming.

[0003] The chemical looping process includes a reduction reactor and an oxidation reactor. The solid material circulating in different reactors of the chemical looping process is called an oxygen carrier. The oxygen carrier is usually reduced in the reduction reactor and oxidized and regenerated in the oxidation reactor. In addition, the chemical looping process usually operates at high temperatures, and the serial fluidized bed reactor is the most commonly used reactor. The physical fluidization characteristics of the oxygen carrier at high temperatures are also the key to the long-term operation of the chemical looping process. Therefore, the development of new oxygen carriers with active chemical properties and stable physical fluidization properties is crucial to the industrialization of the chemical looping process, and the performance of the oxygen carrier needs to be tested.

[0004] At present, oxygen carriers are mainly tested using large serial fluidized bed reactors. This testing process has the following defects: 1. It requires a large amount of oxygen carriers and reaction gases, resulting in a large waste of time and resources; 2. It takes 4-5 people to complete the operation of switching the oxygen carrier between the reduction reactor and the oxidation reactor, which is difficult to operate, has high labor costs and low efficiency; 3. If the oxygen carrier detected does not meet the requirements, the product will definitely be unqualified and must be scrapped, resulting in great waste. Summary of the invention

[0005] In order to solve the technical problems in the background technology, the present invention discloses a fluidized bed device for chemical chain oxygen carrier performance testing and a testing method thereof.

[0006] The present invention provides a fluidized bed device for chemical chain oxygen carrier performance testing, comprising:

[0007] A heating furnace is provided with an oxygen carrier for testing inside. The oxygen carrier is installed in a vertically arranged quartz tube. The heating furnace heats the oxygen carrier to a fluidized state. A raw material inlet is provided at the lower end of the quartz tube, and a finished product outlet is provided at the upper end. The main component of the quartz tube is SiO2, which is chemically stable within the range of 1000°C, and can avoid experimental errors caused by chemical reactions between the metal tube and oxidizing / reducing gases, thereby improving test accuracy.

[0008] an oxidizing gas cylinder, the outlet of which is connected to the raw material inlet via a first pipeline;

[0009] a reducing gas cylinder, the outlet of which is connected to the raw material inlet via a second pipeline;

[0010] The oxidizing gas cylinder and the reducing gas cylinder are connected to the raw material inlet in sequence, so that the oxygen carrier circulates in sequence to perform redox reaction;

[0011] The finished product after the reaction is completed flows out from the finished product outlet.

[0012] The beneficial effects of the above arrangement are: 1. The device can carry out redox reactions simultaneously without transferring the oxygen carrier. The redox reaction can be carried out immediately by switching the oxidizing gas and the reducing gas. It not only has high detection efficiency but also has low labor intensity. 2. Compared with the traditional serial fluidized bed reactor, the device has a simple structure and low cost, and uses less oxygen carrier and reaction gas, which saves time and cost for oxygen carrier performance testing and can significantly improve the efficiency of oxygen carrier performance testing. 3. The device is suitable for the testing and analysis of gas-solid reaction performance in all chemical processes where solids are in a fluidized state.

[0013] When the oxygen carrier switches between oxidation reaction and reduction reaction, the residual gas will affect the reaction of the oxygen carrier, thereby affecting the accuracy of the test results. Based on this, a further improvement is that it also includes an inert gas cylinder, whose outlet is connected to the raw material inlet through a third pipeline; after the oxygen carrier completes the oxidation reaction or the reduction reaction, the inert gas is first filled into the quartz tube to discharge the excess oxidizing gas or reducing gas.

[0014] In order to facilitate the control of the amount of oxidizing gas, reducing gas and inert gas entering the quartz tube, a further design is that flow meters and on-off valves are installed on the first pipeline, the second pipeline and the third pipeline.

[0015] The first pipeline, the second pipeline and the third pipeline are all connected to the raw material inlet, which will lead to a complex structure and difficult installation. Based on this, a further improvement is that the first pipeline, the second pipeline and the third pipeline are collected in an input main pipe, and the outlet end of the input main pipe is connected to the raw material inlet.

[0016] Three on-off valves need to be set up, which is relatively costly and will also make the structure of the pipeline more complicated. Based on this, further improvements are: a four-way valve is installed on the input main pipe to replace the on-off valve; the inlet of the four-way valve is connected to the outlets of the first pipeline, the second pipeline and the third pipeline respectively, and the outlet of the four-way valve is connected to the inlet of the input main pipe.

[0017] The oxygen carrier needs to undergo redox reaction in a fluidized state at a relatively high temperature. If the temperature of the gas input into the quartz tube is too low, the oxygen carrier will solidify, affecting the test results. Based on this, a further improvement is that a preheater is installed on the input main pipe to heat the gas entering the input main pipe.

[0018] The specific installation structure of the oxygen carrier is as follows: the quartz tube is arranged vertically, and the upper quartz wool and the lower quartz wool are arranged in an interval; the oxygen carrier is placed on the lower quartz wool, and there is a gap between the upper quartz wool and the lower quartz wool. The pores of the quartz wool (usually less than 10μm) are smaller than the particle size of the oxygen carrier. The lower quartz wool can prevent the oxygen carrier from leaking from the bottom of the quartz tube while making the reaction gas evenly dispersed. The upper quartz wool can prevent the small particles generated by the oxygen carrier being broken during the test from being carried out of the quartz tube by the reaction gas.

[0019] Since the upper quartz wool is easy to move upward under the action of air pressure and easily detached from the upper end of the quartz tube; the lower quartz wool is easy to descend under the action of gravity and detached from the lower end of the quartz tube, based on this, further improvements are: a lower quartz liner is provided at the lower end of the lower quartz wool; an upper quartz liner is provided at the upper end of the upper quartz wool.

[0020] Furthermore, the finished product outlet is connected to a dust removal dryer and a flue gas analyzer in sequence through pipelines. Fine particles will clog the flue gas analyzer pipeline and affect its service life, and moisture will affect the test accuracy of the flue gas analyzer. The dust removal dryer can remove fine particles in the device pipeline and water generated during the reaction. The flue gas analyzer can measure the concentration of each gas at the outlet of the quartz tube. The change of gas concentration over time reflects the chemical reaction performance of the oxygen carrier.

[0021] The present invention also provides a method for testing a fluidized bed device for chemical chain oxygen carrier performance testing, using a fluidized bed device for chemical chain oxygen carrier performance testing, comprising the following steps:

[0022] S1, oxygen carrier is placed in a quartz tube at room temperature;

[0023] S2. Open the inert gas cylinder to exhaust the air in the quartz tube;

[0024] S3, turning on the heating furnace, raising the temperature to the test temperature, and making the oxygen carrier in a fluidized state;

[0025] S4, close the inert gas cylinder, open the reducing gas cylinder, so that the reducing gas enters the quartz tube and reacts with the oxygen carrier to perform a reduction reaction;

[0026] S5. After the reduction reaction is completed, close the reducing gas cylinder; open the inert gas cylinder, the inert gas enters the quartz tube, and the excess reducing gas in the quartz tube is discharged;

[0027] S6. Close the inert gas cylinder and open the oxidizing gas cylinder, so that the oxidizing gas enters the quartz tube and undergoes an oxidation reaction with the oxygen carrier;

[0028] S7. After the oxidation reaction is completed, close the oxidizing gas cylinder; open the inert gas cylinder, the inert gas enters the quartz tube, and the excess oxidizing gas in the quartz tube is discharged;

[0029] S8, repeating steps S4-S7 until the performance of the oxygen carrier has no significant change;

[0030] S9. Turn off the heating furnace. When the temperature inside the heating furnace drops to room temperature, turn off the inert gas cylinder and the test is finished.

[0031] The beneficial effects of the present invention are: 1. The device can carry out redox reactions simultaneously, and there is no need to transfer the oxygen carrier. The redox reaction can be carried out immediately by switching the oxidizing gas and the reducing gas. Not only is the detection efficiency high, but the labor intensity is also low; 2. Compared with the traditional serial fluidized bed reactor, the device has a simple structure and low cost, and uses less oxygen carrier and reaction gas, which saves time and cost for oxygen carrier performance testing and can significantly improve the efficiency of oxygen carrier performance testing; 3. The device is suitable for testing and analyzing gas-solid reaction performance in all chemical processes where solids are in a fluidized state. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0033] Figure 1 It is a schematic diagram of the structure of the present invention;

[0034] In the figure: 1. Heating furnace; 2. Oxygen carrier; 3. Quartz tube; 4. Oxidizing gas cylinder; 5. Reducing gas cylinder; 6. Inert gas cylinder; 7. Flow meter; 8. Input main pipe; 9. Four-way valve; 10. Preheater; 11. Upper quartz wool; 12. Lower quartz wool; 13. Lower quartz liner; 14. Upper quartz liner; 15. Dust removal dryer; 16. Flue gas analyzer; 31. Raw material inlet; 32. Finished product outlet; 41. First pipeline; 51. Second pipeline; 61. Third pipeline. DETAILED DESCRIPTION

[0035] The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic diagrams, which only illustrate the basic structure of the present invention in a schematic manner, and therefore only show the components related to the present invention.

[0036] Embodiment 1:

[0037] like Figure 1As shown, the present invention discloses a fluidized bed device for chemical chain oxygen carrier performance testing, including a heating furnace 1, in which an oxygen carrier 2 for testing is arranged. The specific installation structure of the oxygen carrier 2 is: a vertically arranged quartz tube 3 is arranged in the heating furnace 1, the upper end of which is a finished product outlet 32, and the lower end is a raw material inlet 31. The oxygen carrier 2 is placed in the quartz tube 3. The main component of the quartz tube 3 is SiO2, which is chemically stable within the range of 1000°C, and can avoid experimental errors caused by chemical reactions between the metal tube and the oxidizing / reducing gas, thereby improving the test accuracy. An upper quartz wool 11 and a lower quartz wool 12 are arranged in an upper and lower interval in the quartz tube 3; the oxygen carrier 2 is placed on the lower quartz wool 12, and a spacing is provided between the oxygen carrier 2 and the upper quartz wool 11 to provide the oxygen carrier 2 with sufficient deformation space. The pores of quartz wool (usually less than 10 μm) are smaller than the particle size of the oxygen carrier. The lower quartz wool 12 can prevent the oxygen carrier 2 from leaking from under the quartz tube 3 while allowing the reaction gas to be evenly dispersed. The upper quartz wool 11 can prevent the small particles generated by the oxygen carrier 2 breaking during the test from being carried out of the quartz tube 3 by the reaction gas.

[0038] Since the upper quartz wool 11 is easy to move upward under the action of air pressure and is easy to detach from the upper end of the quartz tube 3; the lower quartz wool 12 is easy to descend under the action of gravity and detach from the lower end of the quartz tube 3, a lower quartz liner 13 is provided at the lower end of the lower quartz wool 12 for supporting the lower quartz wool 12; an upper quartz liner 14 is provided at the upper end of the upper quartz wool 11 for limiting the upper quartz wool 11.

[0039] The present invention also includes an oxidizing gas cylinder 4, a reducing gas cylinder 5 and an inert gas cylinder 6. The oxidizing gas cylinder 4 is filled with oxidizing gas, and its outlet is connected to the first pipeline 41; the reducing gas cylinder 5 is filled with reducing gas, and its outlet is connected to the second pipeline 51; the inert gas cylinder 6 is filled with inert gas, and its outlet is connected to the third pipeline 61. Flow meters 7 are installed on the first pipeline 41, the second pipeline 51 and the third pipeline 61 to control the output flow of the gas. The first pipeline 41, the second pipeline 51 and the third pipeline 61 are collected in the input main pipe 8, and the outlet of the input main pipe 8 is connected to the raw material inlet 31. Compared with the arrangement in which the outlets of the first pipeline 41, the second pipeline 51 and the third pipeline 61 are all connected to the raw material inlet 31, not only the structure is simple, but also it is easy to install.

[0040] A four-way valve 9 is installed on the input main pipe 8 to control the connection and disconnection between the first pipeline 41, the second pipeline 51, the third pipeline 61 and the raw material inlet 31. Compared with installing an on-off valve on each of the first pipeline 41, the second pipeline 51 and the third pipeline 61, using one four-way valve 9 has a simpler structure and lower cost.

[0041] The oxygen carrier 2 needs to undergo redox reaction in a fluidized state at a relatively high temperature. If the temperature of the gas input into the quartz tube 3 is too low, the oxygen carrier 2 will solidify, affecting the test result. Therefore, a preheater 10 is installed on the input main pipe 8 to heat the gas entering the input main pipe 8.

[0042] The finished product after the reaction flows out from the finished product outlet 32. The finished product outlet 32 ​​is connected to the dust removal dryer 15 and the flue gas analyzer 16 in sequence through pipelines. The dust removal dryer 15 is used to filter the gas flowing out of the finished product outlet 32. Fine particles will block the pipeline of the flue gas analyzer 16 and affect its service life. Water will affect the test accuracy of the flue gas analyzer 16. The dust removal dryer 15 can remove fine particles in the device pipeline and water generated during the reaction. The flue gas analyzer 16 can measure the concentration of each gas at the outlet of the quartz tube 3. The change of gas concentration over time reflects the chemical reaction performance of the oxygen carrier 2.

[0043] The oxidizing gas cylinder 4 and the reducing gas cylinder 5 are sequentially connected to the raw material inlet 31, so that the oxygen carrier 2 circulates the oxidation-reduction reaction in sequence. When the oxygen carrier 2 switches between the oxidation reaction and the reduction reaction, the residual gas will affect the reaction of the oxygen carrier 2, thereby affecting the accuracy of the test result. Therefore, after the oxygen carrier 2 completes the oxidation reaction or the reduction reaction, the quartz tube 3 is first filled with an inert gas to discharge the excess oxidizing gas or reducing gas.

[0044] Compared with the prior art, the beneficial effects of the present invention are: 1. The device can carry out redox reactions simultaneously, and there is no need to transfer the oxygen carrier 2. The redox reaction can be carried out immediately by switching the oxidizing gas and the reducing gas, which not only has high detection efficiency but also has low labor intensity; 2. Compared with the traditional serial fluidized bed reactor, the device has a simple structure and low cost, and uses less oxygen carrier 2 and reaction gas, which saves time and cost for testing the performance of the oxygen carrier 2 and can significantly improve the efficiency of testing the performance of the oxygen carrier 2; 3. The device is suitable for testing and analyzing the gas-solid reaction performance in all chemical processes where solids are in a fluidized state.

[0045] Embodiment 2:

[0046] The present invention also discloses a method for testing a fluidized bed device for chemical chain oxygen carrier performance testing, using the fluidized bed device for chemical chain oxygen carrier performance testing of embodiment 1, comprising the following steps:

[0047] S1, oxygen carrier 2 is placed in quartz tube 3 at room temperature;

[0048] S2, open the inert gas cylinder 6 to exhaust the air in the quartz tube 3;

[0049] S3, start the heating furnace 1, raise the temperature to the test temperature, and make the oxygen carrier 2 in a fluidized state;

[0050] S4, close the inert gas cylinder 6, open the reducing gas cylinder 5, so that the reducing gas enters the quartz tube 3 and performs a reduction reaction with the oxygen carrier 2;

[0051] S5. After the reduction reaction is completed, the reducing gas cylinder 5 is closed; the inert gas cylinder 6 is opened, the inert gas enters the quartz tube 3, and the excess reducing gas in the quartz tube 3 is discharged;

[0052] S6, close the inert gas cylinder 6, open the oxidizing gas cylinder 4, so that the oxidizing gas enters the quartz tube 3 and undergoes an oxidation reaction with the oxygen carrier 2;

[0053] S7, after the oxidation reaction is completed, the oxidizing gas cylinder 4 is closed; the inert gas cylinder 6 is opened, the inert gas enters the quartz tube 3, and the excess oxidizing gas in the quartz tube 3 is discharged;

[0054] S8, repeating steps S4-S7 until the performance of the oxygen carrier 2 has no significant change;

[0055] S9, turn off the heating furnace 1. When the temperature in the heating furnace 1 drops to room temperature, turn off the inert gas cylinder 6, and the test ends.

[0056] The above steps can test the performance of the oxygen carrier 2, which not only has a high test effect but also has accurate test results.

[0057] Based on the above ideal embodiments of the present invention, the relevant staff can make various changes and modifications without departing from the technical concept of the present invention through the above description. The technical scope of the present invention is not limited to the contents of the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A fluidized bed device for chemical chain oxygen carrier performance testing, characterized in that: include: A heating furnace (1) is provided with an oxygen carrier (2) for testing inside, the oxygen carrier (2) being installed in a vertically arranged quartz tube (3), and the heating furnace (1) heats the oxygen carrier (2) to a fluidized state; a raw material inlet (31) is provided at the lower end of the quartz tube (3), and a finished product outlet (32) is provided at the upper end; An oxidizing gas cylinder (4), the outlet of which is connected to the raw material inlet (31) via a first pipeline (41); A reducing gas cylinder (5), the outlet of which is connected to the raw material inlet (31) via a second pipeline (51); The oxidizing gas cylinder (4) and the reducing gas cylinder (5) are sequentially connected to the raw material inlet (31), so that the oxygen carrier (2) circulates sequentially to perform redox reactions; The finished product after the reaction is completed flows out from the finished product outlet (32).

2. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 1, characterized in that: It also includes an inert gas cylinder (6), the outlet of which is connected to the raw material inlet (31) through a third pipeline (61); After the oxygen carrier (2) completes the oxidation reaction or the reduction reaction, the quartz tube (3) is first filled with an inert gas to discharge the excess oxidizing gas or reducing gas.

3. The fluidized bed device for chemical chaining oxygen carrier performance testing according to claim 2, characterized in that: A flow meter (7) and an on-off valve are installed on the first pipeline (41), the second pipeline (51) and the third pipeline (61).

4. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 3, characterized in that: The first pipeline (41), the second pipeline (51) and the third pipeline (61) are connected to an input main pipe (8), and the outlet end of the input main pipe (8) is connected to the raw material inlet (31).

5. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 4, characterized in that: A four-way valve (9) is installed on the input main pipe (8) to replace the on-off valve; the inlet of the four-way valve (9) is respectively connected to the outlets of the first pipeline (41), the second pipeline (51) and the third pipeline (61), and the outlet of the four-way valve (9) is connected to the inlet of the input main pipe (8).

6. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 5, characterized in that: A preheater (10) is installed on the input main pipe (8) to heat the gas entering the input main pipe (8).

7. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 6, characterized in that: The interior of the quartz tube (3) is provided with upper quartz wool (11) and lower quartz wool (12) arranged in an upper and lower interval; The oxygen carrier (2) is placed on the lower quartz wool (12) and a distance is provided between the oxygen carrier (2) and the upper quartz wool (11).

8. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 7, characterized in that: A lower quartz liner (13) is provided at the lower end of the lower quartz wool (12); and an upper quartz liner (14) is provided at the upper end of the upper quartz wool (11).

9. The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 8, characterized in that: The finished product outlet (32) is sequentially connected to a dust removal dryer (15) and a flue gas analyzer (16) through pipelines.

10. A method for testing a fluidized bed device for chemical chain oxygen carrier performance testing, characterized in that: The fluidized bed device for chemical chain oxygen carrier performance testing according to claim 9 comprises the following steps: S1, the oxygen carrier (2) is placed in a quartz tube (3) at room temperature; S2, opening the inert gas cylinder (6) to exhaust the air in the quartz tube (3); S3, starting the heating furnace (1) and heating it to a test temperature so that the oxygen carrier (2) is in a fluidized state; S4, closing the inert gas cylinder (6), and opening the reducing gas cylinder (5), so that the reducing gas enters the quartz tube (3) and undergoes a reduction reaction with the oxygen carrier (2); S5. After the reduction reaction is completed, the reducing gas cylinder (5) is closed; the inert gas cylinder (6) is opened, the inert gas enters the quartz tube (3), and the excess reducing gas in the quartz tube (3) is discharged; S6, closing the inert gas cylinder (6), and opening the oxidizing gas cylinder (4), so that the oxidizing gas enters the quartz tube (3) and undergoes an oxidation reaction with the oxygen carrier (2); S7, after the oxidation reaction is completed, the oxidizing gas cylinder (4) is closed; the inert gas cylinder (6) is opened, the inert gas enters the quartz tube (3), and the excess oxidizing gas in the quartz tube (3) is discharged; S8, repeating steps S4-S7 until the performance of the oxygen carrier (2) has no significant change; S9, closing the heating furnace (1), and when the temperature in the heating furnace (1) drops to room temperature, closing the inert gas cylinder (6), and the test ends.

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