Oxygen carrier abrasion evaluation device and method

Abstract

The invention discloses an oxygen carrier abrasion evaluation device and method. The device comprises a computer, a PLC, a weighing sensor, a differential pressure sensor, a buffer gas chamber, an infrared heating furnace, a compressed gas cylinder, a water storage bottle, a sampling pipe, a tail gas collecting pipe, a filter, a micro gas pump and a reactor. Wherein the computer, the weighing sensor, the differential pressure sensor and the infrared heating furnace are all connected with the PLC, a reactor is arranged in the infrared heating furnace, the weighing sensor is provided with the scale, the scale is provided with the buffer gas chamber, the buffer gas chamber is communicated with the reactor, and the compressed gas cylinder and the water storage cylinder are both connected with the buffer gas chamber; the micro air pump is connected with the filter which is connected with the tail gas collecting pipe. Under the conditions of a mechanical wear experiment and a thermal stress wear experiment, the wear performance of the oxygen carrier is evaluated by drawing a thermogravimetric curve and calculating the wear rate by using a thermogravimetric signal transmitted by the device, which indicates that the oxygen carrier has good chemical looping reaction wear resistance, and the method provides a scientific basis for optimizing the design and operation of a chemical looping reaction system.

Description

Technical Field

[0001] The invention belongs to the technical field of oxygen carrier wear resistance evaluation, and particularly relates to an oxygen carrier wear evaluation device and method. Background Art

[0002] Oxygen carriers play a crucial role in chemical chain reactions, acting as heat carriers, mass transfer agents, and reaction centers. During long-term operation, oxygen carriers are subject to wear and tear. Once wear reaches a certain level, they become unusable, and the chemical chain reaction ceases to proceed. Wear evaluation is a key step in assessing whether oxygen carriers can maintain structural and performance stability over long periods of use.

[0003] Under high-temperature cyclic conditions, oxygen carriers will experience particle breakage, surface peeling, and pore structure degradation due to factors such as mechanical wear, thermal stress wear, and reaction wear, resulting in decreased reaction activity, attenuation of oxygen carrying capacity, and even abnormal fluidization of the system. Wear evaluation has become a key link in assessing whether oxygen carriers can maintain structural and performance stability during long-term use. Usually, by simulating actual operating conditions, the oxygen carriers are circulated for a long time, and then indicators such as particle size changes, breakage rate, and performance attenuation are observed. Wear evaluation is used to screen out oxygen carriers with high mechanical strength and good wear resistance to adapt to different application scenarios. The development of high-performance, wear-resistant oxygen carriers is of great significance to the development of chemical chain reaction technology.

[0004] The screening of high-performance, wear-resistant oxygen carriers is one of the bottlenecks in the industrial application of chemical chaining technology. At present, there is no unified standard for the wear test of oxygen carriers. The literature mostly uses fluidized bed reactors for testing, and the wear is evaluated by analyzing the particle distribution after a period of operation or capturing fine particles entrained out of the bed with the airflow. The main evaluation object of this method is small particle size (such as 0.2mm), and it is difficult to evaluate the wear process caused by particle collision of industrial-grade oxygen carrier particles (such as 3-5mm in diameter and 4-5mm in height). There is an urgent need to develop an industrial-grade oxygen carrier wear evaluation method. Summary of the Invention

[0005] In order to solve the problem in the prior art that it is difficult to evaluate the wear process of industrial-grade oxygen carrier particles, the purpose of the present invention is to provide an oxygen carrier wear evaluation device and method.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] An oxygen carrier wear evaluation device includes a computer, a PLC, a weighing sensor, a pressure differential sensor, a buffer gas chamber, an infrared heating furnace, a compressed gas cylinder, a water storage bottle, a sampling tube, an exhaust gas collection tube, a filter, a micro air pump and a reactor;

[0008] The computer, weighing sensor, differential pressure sensor and infrared heating furnace are all connected to the PLC. A reactor is set in the infrared heating furnace. A weighing pan is set on the weighing sensor. A buffer gas chamber is set on the weighing pan. The buffer gas chamber is connected to the reactor. The compressed gas cylinder and the water storage bottle are both connected to the buffer gas chamber.

[0009] The micro air pump is connected to the filter, and the filter is connected to the tail gas collecting pipe.

[0010] Furthermore, a pressure reducing valve, a mass flow meter, a one-way valve and a three-way valve are provided between the compressed gas cylinder and the buffer gas chamber.

[0011] Furthermore, a sampling tube air inlet is provided at the bottom end of the sampling tube, and a sampling tube air outlet is provided at the top end;

[0012] The tail gas collecting pipe is sleeved on the sampling pipe, the bottom of the tail gas collecting pipe is provided with a tail gas collecting pipe air inlet, the side wall is provided with a tail gas collecting pipe air outlet, and the top is closed.

[0013] Furthermore, the sampling tube air inlet of the sampling tube is inserted into the reactor, and the air inlet of the tail gas collecting tube is connected to the top outlet of the reactor.

[0014] Furthermore, the sampling tube and the exhaust gas collecting tube are arranged on a fixed plate; a screw rod is provided on the fixed plate and fixed by the screw rod.

[0015] Furthermore, the filter is a T-type three-stage filter.

[0016] Furthermore, the filter includes a filter cavity, a spring, a sealing shell and a filter housing; wherein, the micro air pump is connected to one end of the hose, a nut is provided at the other end of the hose, the hose is connected to one end of the filter housing through the nut, a filter cavity is provided in the filter housing, an internal thread is provided on the filter housing, the sealing shell is provided at the bottom of the filter housing, the spring is provided on the bottom surface of the filter cavity, and is located in the sealing shell, and the gas after the reaction in the reactor enters the cavity between the outer wall of the filter housing and the filter cavity.

[0017] Furthermore, the filter cavity includes a primary filter layer, a secondary filter layer and a primary filter layer arranged in sequence from the inside to the outside.

[0018] Furthermore, the primary filter layer is a millimeter-scale metal mesh filter layer, the secondary filter layer is a micron-scale sintered fiber filter layer, and the primary filter layer is a picometer-scale filter layer;

[0019] Among them, the first-level filter layer, the second-level filter layer and the first-level filter layer are arranged on a metal filter support frame, the metal filter support frame is sintered on the filter bottom plate, the filter bottom plate is set on the spring, and the outside of the metal filter support frame of the first-level filter layer is provided with picometer-level folded filter paper.

[0020] A method for evaluating oxygen carrier wear, comprising:

[0021] Oxygen carrier particles are mixed with quartz sand and added to a reactor. The fluidized quartz sand collides with the oxygen carrier to produce wear. After the wear particles are carried away by the gas, a weighing sensor measures the mass of the oxygen carrier and outputs a thermogravimetric signal of the mechanical wear stage. The thermogravimetric signal of the mechanical wear process is processed by a computer into a weight loss curve. The initial ordinate of the weight loss curve is the mass of the oxygen carrier before mechanical wear, and the ordinate at the reaction end point is the mass after wear. The wear rate of the process is calculated based on the difference in mass before and after wear, thereby realizing the evaluation of the mechanical wear performance of the oxygen carrier particles.

[0022] If the wear rate of the oxygen carrier obtained by the mechanical wear test is greater than or equal to 5%, the evaluation is stopped and the wear rate of the oxygen carrier is obtained. If the wear rate of the oxygen carrier obtained by the mechanical wear test is less than 5%, a thermal stress wear test is performed to test the wear rate of the oxygen carrier.

[0023] The thermal stress wear test process is as follows: oxygen carrier particles are mixed with quartz sand and added to a reactor. The reactor is heated to 790-800°C using a PLC-controlled infrared heating furnace. The weight loss curve during the wear process is displayed on a computer. The wear rate is calculated based on the mass difference before and after wear in the oxygen carrier weight loss curve, thereby evaluating the thermal stress wear performance of the oxygen carrier particles.

[0024] If the wear rate of the oxygen carrier measured by the thermal stress wear test is greater than or equal to 5%, the test is stopped to obtain the wear rate of the oxygen carrier. If the wear rate of the oxygen carrier measured by the thermal stress wear test is less than 5%, a reactive wear test is performed to test the wear rate.

[0025] Reactive wear test process: The oxygen carrier particles are mixed with quartz sand, weighed and added to the reactor. The reactor is heated to the reaction temperature using a PLC-controlled infrared heating furnace. The reducing gas used to reduce the oxygen carrier, the inert gas used for purging, the wet inert gas used for the initial oxidation and reduction of the oxygen carrier, the inert gas used for purging, and the oxygen-containing inert gas used to complete deep oxidation are switched in sequence to complete an "oxygen carrier reduction-oxidation" reaction cycle. The fluidized quartz sand collides with the reacting oxygen carrier to produce wear. The wear particles are carried out by the gas and captured by the filter. After the reaction is completed, the mass of the oxygen carrier and quartz sand after wear is weighed, and the wear rate is calculated from the mass difference before and after wear to achieve the evaluation of the reactive wear performance.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] Traditional fluidized bed reactor evaluation methods can only evaluate small-sized particles, but the wear evaluation method of the present invention can evaluate industrial-grade oxygen carrier particles. First, the present invention mixes quartz sand with oxygen carrier particles and adds them to a fluidized bed reactor. By fluidizing the small-sized quartz sand, the oxygen carrier particles, which are difficult to fluidize, are worn away by the large-sized oxygen carrier particles. This method serves as a means of characterizing the mechanical wear of large-sized oxygen carriers, directly expanding the particle size range applicable to fluidized bed reactors in the field of oxygen carrier wear evaluation. Second, because this study uses fluidized quartz sand as a means of mechanically wearing the oxygen carrier particles, the present invention can complete three different levels of wear evaluation: mechanical wear, thermal stress wear, and reaction wear, in the same reactor. Finally, the three types of wear are layered and located in the same reactor, which is more consistent with the actual wear of oxygen carriers in chemical chain reactors, and the resulting wear evaluation is more realistic. A three-stage filter is used as a supplementary device to compensate for the loss of a stable thermogravimetric signal during the reaction wear evaluation process due to frequent gas switching and the inability to output a stable thermogravimetric signal. The particles captured in the three-stage filter are the oxygen carrier particle residues that were worn away during the reaction process. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a schematic diagram of the oxygen carrier wear evaluation of the present invention;

[0029] Figure 2 is a schematic diagram of the oxygen carrier wear evaluation device of the present invention;

[0030] Figure 3 It is a schematic diagram of the filter structure of the present invention;

[0031] Figure 4 Schematic diagram of the filter cavity of the filter of the present invention;

[0032] Figure 5 This is the mechanical wear weight loss curve of the present invention;

[0033] Figure 6 This is the thermal stress wear weight loss curve of the present invention.

[0034] In the figure, 1 is a computer, 2 is a PLC, 3 is a weighing sensor, 4 is a differential pressure sensor, 5 is a buffer gas chamber, 6 is an infrared heating furnace, 7 is a compressed gas cylinder, 8 is a water storage bottle, 9 is a pressure reducing valve, 10 is a mass flow meter, 11 is a one-way valve, 12 is a three-way valve, 13 is the air inlet of the sampling tube, 14 is the air inlet of the exhaust gas collection pipe, 15 is the air outlet of the exhaust gas collection pipe, 16 is a fixing plate, 17 is the air outlet of the sampling tube, 18 is a filter, 19 is a micro air pump, 20 is a screw rod, 21 is a reactor, 22 is a nut, 23 is a filter cavity, 24 is a spring, 25 is a sealing shell, 26 is a filter housing, 27 is a primary filter layer, 28 is a secondary filter layer, 29 is a filter bottom plate, and 30 is a tertiary filter layer. DETAILED DESCRIPTION

[0035] To facilitate understanding of the present invention, the present invention will be described more fully below with reference to the accompanying drawings. The accompanying drawings illustrate preferred embodiments of the present invention. However, the present invention may be implemented in a variety of different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and comprehensive understanding of the disclosure of the present invention.

[0036] In addition, when an element in the present invention is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be an intermediate element. When an element is referred to as being "connected to" another element, it may be directly connected to the other element or there may be an intermediate element. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only implementation method.

[0037] See also Figure 2 The oxygen carrier wear evaluation device of the present invention includes a computer 1, a PLC 2, a weighing sensor 3, a pressure difference sensor 4, a buffer gas chamber 5, an infrared heating furnace 6, a compressed gas cylinder 7, a water storage bottle 8, a pressure reducing valve 9, a mass flow meter 10, a one-way valve 11, a three-way valve 12, a sampling tube, an exhaust gas collection tube, a filter 18, a micro air pump 19, a screw 20 and a reactor 21.

[0038] Among them, the computer 1, the weighing sensor 3, the pressure difference sensor 4, the infrared heating furnace 6, the mass flowmeter 10, the one-way valve 11 and the three-way valve 12 are all connected to the PLC 2. A reactor 21 is set in the infrared heating furnace 6. A weighing pan is set on the weighing sensor 3. A buffer gas chamber 5 is set on the weighing pan. The buffer gas chamber 5 is connected to the reactor 21. The weighing sensor 3 weighs the total weight of the buffer gas chamber 5 and the reactor 21. A pressure reducing valve 9 is installed on the compressed gas cylinder 7. The outlet of the compressed gas cylinder 7 is connected to the buffer gas chamber 5 through a pipeline via the pressure reducing valve 9, the mass flowmeter 10, the one-way valve 11 and the three-way valve 12. The water storage bottle 8 is connected to the buffer gas chamber 5.

[0039] The sampling tube and the tail gas collecting tube are arranged on the fixing plate 16 and fixed by the fixing plate 16 . The fixing plate 16 is fixed by the screw rod 20 , and one end of the screw rod 20 is fixed at a set position.

[0040] The bottom end of the sampling tube is provided with a sampling tube air inlet 13 , and the top end of the sampling tube is provided with a sampling tube air outlet 17 .

[0041] The exhaust collection tube is mounted on the sampling tube. It has an exhaust collection tube air inlet 14 at its bottom and an exhaust collection tube air outlet 15 on its sidewall. The top is sealed. A micro air pump 19 is connected to a filter 18 via a hose. The filter 18 is connected to the exhaust collection tube air inlet 14.

[0042] The sampling tube air inlet 13 of the sampling tube is inserted into the reactor 21 , the tail gas collection tube air inlet 14 is located outside the reactor 21 and is connected to the top outlet of the reactor 21 , and the sampling tube air inlet 13 is lower than the tail gas collection tube air outlet 14 .

[0043] See also Figure 3 , the filter 18 is a T-type three-stage filter. The filter 18 includes a nut 22, a filter cavity 23, a spring 24, a sealing shell 25 and a filter housing 26. Among them, a nut 22 is provided at the end of the hose, and the hose is connected to one end of the filter housing 26 through the nut 22. The filter cavity 23 is provided in the filter housing 26, and the filter housing 26 is provided with an internal thread. The sealing shell 25 is provided at the bottom of the filter housing 26 and the sealing shell 25 is connected to the filter housing 26 through a thread. The spring 24 is provided on the bottom surface of the filter cavity 23 and is located in the sealing shell 25, supporting the filter cavity 23. The hose is connected to the filter housing 26 by an internal thread through the nut 22. The reacted gas (i.e., the gas containing wear particles) enters the filter housing 26, and then enters the cavity between the outer wall of the filter housing 26 and the filter cavity 23.

[0044] See also Figure 4 The filter chamber 23 includes, from the inside out, a tertiary filter layer 30, a secondary filter layer 28, and a primary filter layer 27. The primary filter layer 27 is a millimeter (mm) metal mesh filter layer, the secondary filter layer 28 is a micron (μm) sintered fiber filter layer, and the tertiary filter layer 30 is a picometer (pm) filter layer. The tertiary filter layer 30, secondary filter layer 28, and primary filter layer 27 are mounted on corresponding metal filter mesh supports. The metal filter mesh supports are sintered together on a filter base plate 29, which is mounted on a spring 24. PM-grade pleated filter paper is attached to the outside of the metal filter mesh support of the tertiary filter layer 30. The gas containing wear particles enters the cavity between the primary filter layer 27 and the filter housing 26 through the hose, then passes through the primary filter layer 27, the secondary filter layer 28 and the tertiary filter layer 30, enters the tertiary filter layer 30, and is discharged from the top of the tertiary filter layer 30, and then discharged through the micro air pump 19. The wear particles are sequentially retained outside the filter layers according to the particle size grades of mm, μm and pm, thereby realizing the graded capture of wear particles.

[0045] The oxygen carrier particle wear evaluation method of the present invention is a thermogravimetric test method, which is carried out through mechanical wear test, thermal stress wear test and reaction wear test. The wear rate of the oxygen carrier is calculated using formula (1) based on the weight loss curve of the thermogravimetric test to complete the evaluation of the wear performance of the oxygen carrier.

[0046]

[0047] The following details the specific process of three different levels of wear:

[0048] The process of the mechanical wear experiment is as follows: the oxygen carrier particles are mixed with quartz sand and added to the reactor 21. The fluidized quartz sand collides with the oxygen carrier to produce wear. After the wear particles are carried away by the gas, the mass of the oxygen carrier will decrease with the passage of time. This change is measured by the weighing sensor 3 and output as a thermogravimetric signal of the mechanical wear stage. The thermogravimetric signal of the mechanical wear process is processed into a weight loss curve by the computer 1. The initial vertical coordinate of the weight loss curve is the mass of the oxygen carrier before mechanical wear, and the vertical coordinate of the reaction end point is the mass after wear. The wear rate of the process can be calculated based on the difference in mass before and after wear, thereby realizing the evaluation of the mechanical wear performance of the oxygen carrier particles. The specific steps are as follows:

[0049] Step 1: Weigh 2-3g of quartz sand and 2-3g of oxygen carrier, mix them and add them to the reactor 21;

[0050] Step 2: Open the compressed gas cylinder 7 and use Ar as the fluidizing gas. The gas velocity at which the quartz sand is just fluidized is the minimum fluidizing gas velocity.

[0051] In step three, the fluidized quartz sand collides with the oxygen carrier to produce wear, and the wear is ventilated at room temperature for 2-3 hours; the mass of the oxygen carrier will decrease with the passage of time, and this change is measured by the weighing sensor 3 and output as a thermogravimetric signal of the mechanical wear stage. The thermogravimetric signal of the mechanical wear process is processed by the computer 1 into a weight loss curve.

[0052] Step 4: The initial ordinate of the weight loss curve is the mass of the oxygen carrier before mechanical wear, and the ordinate at the reaction end point is the mass after wear. The wear rate of the process can be calculated based on the difference in mass before and after wear, thereby realizing the evaluation of the mechanical wear performance of the oxygen carrier particles.

[0053] If the wear rate of the oxygen carrier obtained by the mechanical wear test is greater than or equal to 5%, the evaluation is stopped, that is, the wear rate of the oxygen carrier is obtained. If the wear rate of the oxygen carrier obtained by the mechanical wear test is less than 5%, a thermal stress wear test is performed to test the wear rate of the oxygen carrier.

[0054] The thermal stress wear test process is as follows: oxygen carrier particles are mixed with quartz sand and added to reactor 21. Infrared heating furnace 6, controlled by PLC2, is used to heat reactor 21 to 790-800°C. The fluidized quartz sand collides with the oxygen carrier, causing wear. The wear particles are carried away by the gas. A weight loss curve during the wear process is displayed by computer 1. The wear rate is calculated based on the mass difference before and after wear in the oxygen carrier weight loss curve, thereby evaluating the thermal stress wear performance of the oxygen carrier particles. The specific steps are as follows:

[0055] Step 1: Weigh 2-3g of quartz sand and 2-3g of oxygen carrier, mix them, and add them to the reactor;

[0056] Step 2: Open the compressed gas cylinder 7 and use Ar as the fluidizing gas. The gas velocity at which the quartz sand is just fluidized is the minimum fluidizing gas velocity.

[0057] Step 3: PLC 2 controls an infrared heating furnace to heat reactor 21 to 790-800°C at a heating rate of 55-60°C / min and maintain the temperature for 2-3 hours to allow the oxygen carrier to undergo thermal stress wear. The fluidized quartz sand collides with the oxygen carrier, causing wear. The wear particles are carried away by the gas, and the weight loss curve during the wear process is displayed by computer 1.

[0058] Step 4: Calculate the wear rate based on the mass difference before and after wear in the oxygen carrier weight loss curve, thereby evaluating the thermal stress wear performance of the oxygen carrier particles.

[0059] If the wear rate of the oxygen carrier measured by the thermal stress wear test is greater than or equal to 5%, the test is stopped to obtain the wear rate of the oxygen carrier. If the wear rate of the oxygen carrier measured by the thermal stress wear test is less than 5%, a reactive wear test is performed to test the wear rate.

[0060] Reaction wear experiment process: The oxygen carrier particles are mixed with quartz sand, weighed and added to the reactor 21, and the reactor 21 is heated to the reaction temperature using the infrared heating furnace 6 controlled by PLC 2. The reducing gas used to reduce the oxygen carrier, the inert gas used for purging, the wet inert gas used for the initial oxidation and reduction of the oxygen carrier, the inert gas used for purging, and the oxygen-containing inert gas used to complete the deep oxidation are switched in sequence to complete an "oxygen carrier reduction-oxidation" reaction cycle. The fluidized quartz sand collides with the reacting oxygen carrier to produce wear, and the wear particles are carried out by the gas and captured by the filter 18. After the reaction is completed, the mass of the oxygen carrier and quartz sand after wear is weighed, and the wear rate is calculated based on the mass difference before and after wear to achieve the evaluation of the reaction wear performance. The specific steps are as follows:

[0061] Step 1: Weigh 2-3g of quartz sand and 2-3g of oxygen carrier, mix them and add them to the reactor 21;

[0062] Step 2: Add argon and raise the reactor to a predetermined temperature;

[0063] Step 3: Add reducing gas for 10-15 minutes to allow the oxygen carrier to complete the deoxygenation reaction;

[0064] Step 4: introduce argon and purge for 4-5 minutes;

[0065] Step 5: purging argon to bring water vapor into the reactor 21 for 10-15 minutes, and the oxygen carrier particles complete the first oxidation reaction;

[0066] Step 6: Introduce argon and purge for 4-5 minutes;

[0067] Step 7: A mixture of argon and oxygen (the volume percentage of oxygen is 4%-5%) is introduced for 10-15 minutes to allow the oxygen carrier particles to complete the oxidation reaction and regain their oxidation capacity;

[0068] Step 8: Introduce argon and purge for 4-5 minutes;

[0069] Step 9: Collect the damaged oxygen carrier residue in the filter 18;

[0070] Step 10: Weigh the mass of the oxygen carrier after the reaction, calculate the wear rate based on the mass difference, and evaluate the reactive wear performance of the oxygen carrier.

[0071] Example 1

[0072] Mechanical wear test:

[0073] Evaluation sample: 2 g of quartz sand (150-180 μm) and 2 g of oxygen carrier (3-5 mm).

[0074] Evaluation method: Quartz sand is mixed with an oxygen carrier, added to a reactor, and abraded at a gas velocity of 0.4 m / s for 3 hours. The fluidized quartz sand collides with the oxygen carrier to produce wear, and the wear particles are carried away by the gas. The thermogravimetric signal during the wear process is processed by computer 1 into a weight loss curve of the oxygen carrier. Based on the weight loss curve, the mass difference before and after wear is obtained, the wear rate is calculated, and the mechanical wear performance of the oxygen carrier is evaluated.

[0075] Mechanical wear weight loss curve is as follows Figure 5 As shown, from Figure 5 It can be seen that the oxygen carrier loses 0.019 g of mass at a gas velocity of 0.4 m / s, and the wear rate of mechanical wear is 0.475%, which is <5%. The oxygen carrier passes the evaluation on the mechanical wear level, and the wear rate of the oxygen carrier is 0.475%.

[0076] Example 2

[0077] Thermal stress wear test:

[0078] Evaluation sample: 2 g of quartz sand (150-180 μm) and 2 g of oxygen carrier (3-5 mm).

[0079] Evaluation method: The oxygen carrier is mixed with quartz sand and added to the reactor. The temperature of the reactor is raised to 790-800°C using a PLC-controlled infrared heating furnace. At this temperature, the fluidized quartz sand collides with the oxygen carrier to produce wear, and the wear particles are carried away by the gas. The weight loss curve during the wear process is displayed by computer 1. The wear rate is calculated based on the mass difference before and after wear in the oxygen carrier weight loss curve to evaluate the thermal stress wear performance of the oxygen carrier.

[0080] Thermal stress wear weight loss curve is as follows Figure 6 As shown, from Figure 6 It can be seen that the mass loss is 0.02g at 800℃ and 0.4m / s gas velocity. The wear rate is calculated by formula (1). The calculated wear rate of thermal stress wear is 0.50%, <5%. The thermal stress wear evaluation of the oxygen carrier is passed, and the wear rate of the oxygen carrier is 0.50%.

[0081] Example 3

[0082] Reactive wear test:

[0083] Evaluation sample: 2g quartz sand (150-180μm) and 2g oxygen carrier particles (3-5mm);

[0084] Evaluation method: The oxygen carrier quartz sand is weighed and mixed before being added to the reactor. The reactor is heated to 890-900°C using a PLC-controlled infrared heating furnace. A reducing gas is introduced to reduce the oxygen carrier for 10-15 minutes, followed by argon purge. Wet argon gas flowing through a water tank is then introduced for 10-15 minutes to complete the first oxidation reaction of the oxygen carrier. After switching to argon purge, argon containing 4%-5% oxygen is introduced to complete the deep oxidation reaction of the oxygen carrier. During the reaction, the quartz sand particles remain in a fluidized state. The fluidized quartz sand collides with the oxygen carrier during the reaction, causing wear. The fine powder particles produced during the wear process are carried into the filter through the exhaust collection tube for collection. After the reactor cools to room temperature, the oxygen carrier and quartz sand mixture is weighed. The wear rate is calculated based on the mass difference before and after the reaction to evaluate the wear performance of the oxygen carrier reaction.

[0085] The mass of the oxygen carrier before the reaction was 2.0153 g, the mass of the quartz sand was 2.0557 g, and the mass of the mixture of the oxygen carrier and quartz sand after the reaction was 3.9327 g. The reaction was carried out at 890-900 ° C, and the mass loss after completing one "oxygen carrier reduction-oxidation" cycle was 0.1383 g. The wear rate was 3.40%, which was <5%. The oxygen carrier reaction wear evaluation passed, and the wear rate of the oxygen carrier was 3.40%.

[0086] The foregoing description is merely a description of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the claims. The present invention is not limited to the foregoing embodiments, and variations in the specific structure are permitted. Any variations within the scope of the independent claims of the present invention are also within the scope of protection of the present invention.

[0087] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

Claims

1. An oxygen carrier wear evaluation device, characterized in that: The device comprises a computer (1), a PLC (2), a weighing sensor (3), a differential pressure sensor (4), a buffer gas chamber (5), an infrared heating furnace (6), a compressed gas cylinder (7), a water storage bottle (8), a sampling tube, an exhaust gas collection tube, a filter (18), a micro air pump (19) and a reactor (21); The computer (1), the weighing sensor (3), the differential pressure sensor (4) and the infrared heating furnace (6) are all connected to the PLC (2); a reactor (21) is provided in the infrared heating furnace (6); a weighing pan is provided on the weighing sensor (3); a buffer air chamber (5) is provided on the weighing pan; the buffer air chamber (5) is connected to the reactor (21); and a compressed gas cylinder (7) and a water storage bottle (8) are both connected to the buffer air chamber (5); The micro air pump (19) is connected to the filter (18), and the filter (18) is connected to the tail gas collection pipe.

2. The oxygen carrier wear evaluation device according to claim 1, characterized in that: A pressure reducing valve (9), a mass flow meter (10), a one-way valve (11) and a three-way valve (12) are provided between the compressed gas cylinder (7) and the buffer gas chamber (5).

3. The oxygen carrier wear evaluation device according to claim 1, characterized in that: The bottom end of the sampling tube is provided with a sampling tube air inlet (13), and the top end is provided with a sampling tube air outlet (17); The tail gas collecting pipe is sleeved on the sampling pipe, the bottom of the tail gas collecting pipe is provided with a tail gas collecting pipe air inlet (14), the side wall is provided with a tail gas collecting pipe air outlet (15), and the top end is closed.

4. The oxygen carrier wear evaluation device according to claim 3, characterized in that: The sampling tube air inlet (13) of the sampling tube is inserted into the reactor (21), and the tail gas collection tube air inlet (14) is connected to the top outlet of the reactor (21).

5. The oxygen carrier wear evaluation device according to claim 1, characterized in that: The sampling tube and the tail gas collecting tube are arranged on a fixed plate (16); a screw rod (20) is arranged on the fixed plate (16) and fixed by the screw rod (20).

6. The oxygen carrier wear evaluation device according to claim 1, characterized in that: The filter (18) is a T-type three-stage filter.

7. The oxygen carrier wear evaluation device according to claim 1, characterized in that: The filter (18) comprises a filter cavity (23), a spring (24), a sealing shell (25) and a filter housing (26); wherein the micro air pump (19) is connected to one end of a hose, a nut (22) is provided at the other end of the hose, and the hose is connected to one end of the filter housing (26) through the nut (22); the filter cavity (23) is provided in the filter housing (26), an internal thread is provided on the filter housing (26), the sealing shell (25) is provided at the bottom of the filter housing (26), the spring (24) is provided on the bottom surface of the filter cavity (23) and is located in the sealing shell (25), and the gas after the reaction in the reactor (21) enters the cavity between the outer wall of the filter housing (26) and the filter cavity (23).

8. The oxygen carrier wear evaluation device according to claim 7, characterized in that: The filter cavity (23) comprises a third-level filter layer (30), a second-level filter layer (28) and a first-level filter layer (27) which are arranged in sequence from the inside to the outside.

9. The oxygen carrier wear evaluation device according to claim 8, characterized in that: The first filter layer (27) is a millimeter-level metal mesh filter layer, the second filter layer (28) is a micron-level sintered fiber filter layer, and the third filter layer (30) is a picometer-level filter layer; Among them, the tertiary filter layer (30), the secondary filter layer (28) and the primary filter layer (27) are arranged on a metal filter support frame, the metal filter support frame is sintered on a filter base plate (29), the filter base plate (29) is arranged on a spring (24), and a picometer-level folded filter paper is arranged on the outside of the metal filter support frame of the tertiary filter layer (30).

10. A method for evaluating oxygen carrier wear based on the device according to any one of claims 1 to 9, characterized in that: include: Oxygen carrier particles are mixed with quartz sand and added to a reactor (21). Fluidized quartz sand collides with the oxygen carrier to produce wear. After the wear particles are carried away by the gas, a weighing sensor (3) measures the mass of the oxygen carrier and outputs a thermogravimetric signal of the mechanical wear stage. The thermogravimetric signal of the mechanical wear process is processed into a weight loss curve by a computer (1). The initial ordinate of the weight loss curve is the mass of the oxygen carrier before mechanical wear, and the ordinate at the reaction end point is the mass after wear. The wear rate of the process is calculated based on the difference between the mass before and after wear, thereby realizing the evaluation of the mechanical wear performance of the oxygen carrier particles. If the wear rate of the oxygen carrier obtained by the mechanical wear test is greater than or equal to 5%, the evaluation is stopped and the wear rate of the oxygen carrier is obtained. If the wear rate of the oxygen carrier obtained by the mechanical wear test is less than 5%, a thermal stress wear test is performed to test the wear rate of the oxygen carrier. The process of the thermal stress wear test is as follows: oxygen carrier particles are mixed with quartz sand and added to a reactor (21); the reactor (21) is heated to 790-800°C using an infrared heating furnace (6) controlled by a PLC (2); a weight loss curve during the wear process is displayed by a computer (1); and the wear rate is calculated based on the mass difference before and after wear in the oxygen carrier weight loss curve, thereby realizing the evaluation of the thermal stress wear performance of the oxygen carrier particles; If the wear rate of the oxygen carrier measured by the thermal stress wear test is greater than or equal to 5%, the test is stopped to obtain the wear rate of the oxygen carrier. If the wear rate of the oxygen carrier measured by the thermal stress wear test is less than 5%, a reactive wear test is performed to test the wear rate. Reaction wear test process: oxygen carrier particles are mixed with quartz sand, weighed and added to the reactor (21), and the reactor (21) is heated to the reaction temperature using an infrared heating furnace (6) controlled by a PLC (2). The reducing gas for reducing the oxygen carrier, the inert gas for purging, the wet inert gas for the oxygen carrier after preliminary oxidation and reduction, the inert gas for purging and the oxygen-containing inert gas for completing deep oxidation are switched in sequence to complete an "oxygen carrier reduction-oxidation" reaction cycle. The fluidized quartz sand collides with the reacting oxygen carrier to produce wear. The wear particles are carried out by the gas and captured by the filter (18). After the reaction is completed, the mass of the oxygen carrier and quartz sand after wear is weighed, and the wear rate is calculated based on the mass difference before and after wear to achieve the evaluation of the reaction wear performance.

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