Gas-solid reaction device and gas-solid reaction method

Abstract

The invention provides a gas-solid reaction device and a gas-solid reaction method, and relates to the technical field of reaction equipment, the gas-solid reaction device comprises a riser reaction assembly, a downer reaction assembly and a separation circulation assembly, the riser reaction assembly comprises a pre-reaction section and a riser section; the downer reaction assembly comprises a downer, and the downer is communicated with the lifting pipe; the separation circulation assembly comprises an axial-flow type gas-solid separator, a material storage accompanying bed and a connecting pipeline, an inlet of the axial-flow type gas-solid separator is communicated with an outlet of the downer, a gas phase outlet of the axial-flow type gas-solid separator is communicated with a gas phase area of the material storage accompanying bed, and a solid phase outlet of the axial-flow type gas-solid separator is communicated with a material storage area of the material storage accompanying bed. According to the invention, the riser reaction assembly and the downer reaction assembly are arranged, so that the gas-solid reaction of ultrafine particles mainly occurs in the dilute-phase bed section, the contact and mixing efficiency between gas and solid is effectively enhanced, and the common problems of insufficient gas-solid contact, adhesion between particles, heat exchange dead zone and the like in the dense-phase bed section are avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction equipment, and in particular to a gas-solid reaction device and a gas-solid reaction method. Background Art

[0002] Geldart C particles, also known as ultrafine particles, usually have a particle size of less than 20 μm. Due to the strong van der Waals and electrostatic forces between ultrafine particles, agglomeration, channeling or slugging are prone to occur during the fluidization process, which seriously affects the stability of the fluidized bed operation, thereby limiting the application of ultrafine particles in the fluidized bed field. However, with the continuous development of petroleum refining, chemical industry, material preparation and other fields, it is becoming more and more important to improve the fluidization state of ultrafine particles and apply them to the preparation of chemical products. Chemical vapor deposition (CVD) is a typical powder reaction and preparation technology, which is widely used in the preparation process of photovoltaic materials such as polycrystalline silicon, carbon silicon anode, and silicon carbide. However, there are some common problems in the existing chemical vapor deposition application cases, such as the wall reaction of the raw gas inside the reactor, the existence of heat exchange dead zones in the reactor, and the adhesion between the deposited particles. Fluidized bed reactors have many advantages such as high mass and heat transfer efficiency, uniform internal temperature distribution, intense gas-solid mixing, and large operational flexibility. In recent years, the industry has combined fluidization technology with chemical vapor deposition and gradually applied it to existing chemical vapor deposition processes in an attempt to solve the above problems.

[0003] For example, Chinese patent document CN1198962A discloses a fluidized bed reactor for gas-solid phase processing of ultrafine particles. Although it improves the problem of agglomeration of ultrafine particles during flow to a certain extent, the setting of a large number of internal components will significantly increase the risk of wall adhesion reaction, and there is a lack of specific implementation measures for gas-solid separation in the downstream production. Chinese invention patent CN114850283B discloses a fluidized reaction system coated with ultrafine particles. In this patent document, the deposition carrier and the deposition raw gas still exist in a dense phase bed type in the bottom of the product tank and other areas; at this time, even if a mechanical stirring paddle is set, it is still difficult to avoid problems such as adhesion between particles and uneven temperature distribution in this area; at the same time, the gas-solid flow in the lifting pipe is usually a ring-core structure, and the traditional bottom feeding method will aggravate the adhesion problem of particles at the side wall of the lifting pipe; in addition, the traditional cyclone separator has a low separation efficiency for ultrafine particles, and the dust removal method of the traditional cyclone separator coupled with the filter will significantly reduce the stable operation time of the overall device. Chinese patent document CN117721434A discloses a reactor and method for vapor deposition of ultrafine particles. The above patent improves the fluidized bed state of the main reaction area from a dense phase bed to a dilute phase bed, effectively strengthening the gas-solid mixing in this area and improving the adhesion problem between particles; however, the ultra-short and fast gas-solid separation structure has a relatively low particle size efficiency for ultrafine particles, and the patent also lacks further treatment measures for residual particles. Therefore, it is urgent to solve the technical problems of low gas-solid mixing efficiency, many reaction dead zones, and subsequent separation difficulties in the existing process. Summary of the invention

[0004] In order to overcome the above-mentioned defects of the prior art, the technical problem to be solved by the embodiments of the present invention is to provide a gas-solid reaction device and a gas-solid reaction method for solving at least one of the above-mentioned technical problems.

[0005] The above-mentioned object of the present invention can be achieved by adopting the following technical scheme. The present invention provides a gas-solid reaction device, comprising:

[0006] A riser reaction assembly, the riser reaction assembly comprising a pre-reaction section and a riser section connected to an outlet of the pre-reaction section;

[0007] A downer bed reaction assembly, the downer bed reaction assembly comprises a downer bed, the downer bed and the riser pipe section are arranged side by side, and the inlet of the downer bed is connected with the outlet of the riser pipe section through a bend pipe;

[0008] A separation circulation component, the separation circulation component comprises an axial flow gas-solid separator, a storage companion bed, and a connecting pipeline connecting the outlet of the storage companion bed and the inlet of the pre-reaction section, the connecting pipeline is provided with a fluidizing gas inlet, the inlet of the axial flow gas-solid separator is connected to the outlet of the descending bed, the gas phase outlet of the axial flow gas-solid separator is connected to the gas phase area of ​​the storage companion bed through a purified gas discharge pipe, and the solid phase outlet of the axial flow gas-solid separator is connected to the storage area of ​​the storage companion bed through a captured particle discharge pipe.

[0009] In a preferred embodiment of the present invention, the radial dimension of the pre-reaction section is larger than the radial dimension of the lifting pipe section, and a first diameter reduction structure is provided between the pre-reaction section and the lifting pipe section; and / or, the radial dimension of the pre-reaction section is larger than the radial dimension of the connecting pipeline, and a first diameter expansion structure is provided between the pre-reaction section and the connecting pipeline; and / or, the radial dimension of the down-going bed is larger than the radial dimension of the elbow, and a second diameter expansion structure is provided between the down-going bed and the elbow; and / or, the radial dimension of the down-going bed is larger than the radial dimension of the axial flow gas-solid separator, and a second diameter reduction structure is provided between the down-going bed and the axial flow gas-solid separator.

[0010] In a preferred embodiment of the present invention, the gas-solid reaction device also includes at least one diffusion distributor arranged in the pre-reaction section, the outlet of the connecting pipeline is connected to the diffusion distributor, and the diffusion distributor includes an outlet surface provided with diffusion holes, and the porosity of the outlet surface is 5% to 50%.

[0011] In a preferred embodiment of the present invention, the gas-solid reaction device also includes a first ring pipe distributor arranged in the pre-reaction section, the first ring pipe distributor is horizontally arranged and placed upstream of the diffusion distributor; and / or, the gas-solid reaction device also includes a second ring pipe distributor arranged in the material storage companion bed, the second ring pipe distributor is horizontally arranged and placed at the bottom of the material storage companion bed.

[0012] In a preferred embodiment of the present invention, the ratio of the diameter of the pre-reaction section to the diameter of the riser section is 1.2 to 3; and / or the bending radius R of the elbow and the diameter of the elbow are 0.5 to 10; and / or the ratio of the diameter of the downcomer to the diameter of the pre-reaction section is 0.5 to 3.

[0013] In a preferred embodiment of the present invention, along the circumference of the pre-reaction section, at least one row of first gas-phase feed hole groups are provided on the pre-reaction section; and / or, along the circumference of the riser section, at least one row of second gas-phase feed hole groups are provided on the riser section; and / or, along the circumference of the downer, at least one row of third gas-phase feed hole groups are provided on the downer.

[0014] In a preferred embodiment of the present invention, the first gas-phase feed hole group includes at least one first gas-phase feed hole arranged on the pre-reaction section along the height direction, and a first gas-phase nozzle arranged on each of the first gas-phase feed holes, and the angle between the incident direction of the first gas-phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section is 10° to 170°; and / or, the second gas-phase feed hole group includes at least one second gas-phase feed hole arranged on the riser section along the height direction, and a second gas-phase nozzle arranged on each of the second gas-phase feed holes, and the angle between the incident direction of the second gas-phase nozzle and the movement direction of the multiphase fluid in the riser section is 10° to 170°; and / or, the third gas-phase feed hole group includes at least one third gas-phase feed hole arranged on the down-bed along the height direction, and a third gas-phase nozzle arranged on each of the third gas-phase feed holes, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed is 10° to 170°.

[0015] In a preferred embodiment of the present invention, the gas-solid reaction device further comprises a dust-containing gas filtering assembly disposed on the top of the storage bed.

[0016] In a preferred embodiment of the present invention, the gas-solid reaction device further comprises a discharge valve arranged at the bottom of the material storage companion bed, and a discharge valve arranged at the outlet of the material storage companion bed.

[0017] The present invention also provides a gas-solid reaction method, which is implemented by using the aforementioned gas-solid reaction device, and the gas-solid reaction method comprises the following steps:

[0018] Close the discharge valve and start the gas phase supply of the second ring pipe distributor to make the ultrafine particles in the storage bed flow;

[0019] Open the feed valve and the fluidizing gas inlet at the same time to introduce fluidizing gas and feed gas into the connecting pipeline to transport ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly within the entrained gas range;

[0020] Opening the first annular distributor to introduce supplementary fluidizing gas into the pre-reaction section to avoid formation of a flow dead zone at the bottom of the pre-reaction section;

[0021] During the reaction of the ultrafine particles, fluidizing gas and raw material gas are introduced into the riser reaction assembly and / or the downer reaction assembly to maintain the raw material gas concentration in the reaction assembly; wherein the raw material gas injection velocity in the riser reaction assembly and / or the downer reaction assembly is 10 m / s to 100 m / s;

[0022] After the ultrafine particles have reacted in the riser reaction assembly and the downer reaction assembly in sequence, the multiphase fluid output from the downer is separated by an axial flow gas-solid separator, the separated ultrafine particles are transported back to the storage companion bed to continue to participate in the circulation, and the separated gas phase fluid is transported back to the storage companion bed and discharged after being filtered;

[0023] When the ultrafine particles complete the reaction cycle, the feed valve is closed to stop the cycle, and the discharge valve is opened to discharge the ultrafine particles.

[0024] The technical solution of the present invention has the following significant beneficial effects:

[0025] The gas-solid reaction device of the present invention is suitable for ultrafine particles. By setting a riser reaction component and a descending bed reaction component, the gas-solid reaction of ultrafine particles mainly occurs in the dilute phase bed section, effectively enhancing the contact and mixing efficiency between gas and solid, and avoiding the common problems of insufficient gas-solid contact, adhesion between particles, and heat exchange dead zone in the dense phase bed section. In addition, by expanding the diameter of the descending bed, not only the agglomeration phenomenon of ultrafine particles during the flow process is significantly reduced, but also the solid phase concentration in the descending bed is moderately increased, further improving the gas-solid contact and mixing efficiency. In addition, an axial flow gas-solid separator is configured at the end of the descending bed to achieve fast and efficient gas-solid separation, reduce the burden of subsequent filtering components, and optimize the stable operation cycle of the entire device. By making the riser reaction component, the descending bed reaction component and the separation circulation component form a circulation pipeline, the total reaction time of the solid phase can be adjusted as needed, thereby enhancing the flexibility of operation. The gas-solid reaction device also has the advantages of saving space and large operational flexibility, and improves the reaction efficiency and system reliability as a whole. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0027] The accompanying drawings described herein are only for explanation purposes and are not intended to limit the scope of the present invention in any way. In addition, the shapes and proportional dimensions of the various components in the figures are only schematic, used to help understand the present invention, and are not specifically limited to the shapes and proportional dimensions of the various components of the present invention. Those skilled in the art can select various possible shapes and proportional dimensions to implement the present invention according to the teachings of the present invention.

[0028] Figure 1 It is a schematic structural diagram of an embodiment of the gas-solid reaction device of the present invention.

[0029] Reference numerals of the above drawings:

[0030] 1. Riser reaction assembly; 11. First expansion structure; 111. First ring pipe distributor; 112. Diffusor distributor; 12. Pre-reaction section; 120. First gas-phase feed hole group; 121. First gas-phase feed hole; 13. First reduction structure; 14. Riser section; 140. Second gas-phase feed hole group; 141. Second gas-phase feed hole;

[0031] 2. Bend pipe;

[0032] 3. Downward bed reaction assembly; 31. Second diameter expansion structure; 32. Downward bed; 320. Third gas phase feed hole group; 321. Third gas phase feed hole; 33. Second diameter reduction structure;

[0033] 4. Separation circulation component; 41. Axial flow gas-solid separator; 42. Separation pipeline; 421. Purified gas discharge pipe; 422. Collected particle discharge pipe; 43. Storage bed; 44. Filter component; 45. Discharge valve; 46. Second ring pipe distributor; 47. Unloading valve; 48. Fluidizing gas inlet; 49. Connecting pipeline. DETAILED DESCRIPTION

[0034] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0035] Implementation Method 1

[0036] Please refer to Figure 1As shown, a gas-solid reaction device is provided in an embodiment of the present invention, which at least comprises a riser reaction assembly 1, a downer reaction assembly 3 and a separation circulation assembly 4, wherein the riser reaction assembly 1 comprises a pre-reaction section 12 and a riser section 14 connected to the outlet of the pre-reaction section 12; the downer reaction assembly 3 comprises a downer 32, the downer 32 and the riser section 14 are arranged side by side, and the inlet of the downer 32 is connected to the outlet of the riser section 14 through a bend 2; the separation circulation assembly 4 comprises an axial A flow-type gas-solid separator 41, a storage companion bed 43, and a connecting pipeline 49 connecting the outlet of the storage companion bed 43 and the inlet of the pre-reaction section 12, the connecting pipeline 49 is provided with a fluidizing gas inlet 48, the inlet of the axial-flow gas-solid separator 41 is connected to the outlet of the down-going bed 32, the gas phase outlet of the axial-flow gas-solid separator 41 is connected to the gas phase area of ​​the storage companion bed 43 through the purified gas discharge pipe 421, and the solid phase outlet of the axial-flow gas-solid separator 41 is connected to the storage area of ​​the storage companion bed 43 through the captured particle discharge pipe 422.

[0037] On the whole, the gas-solid reaction device of the present invention is suitable for ultrafine particles. By setting up the riser reaction component 1 and the down-bed reaction component 3, the gas-solid reaction of ultrafine particles mainly occurs in the dilute bed section, which effectively enhances the contact and mixing efficiency between gas and solid, and avoids the common problems of insufficient gas-solid contact, adhesion between particles, and heat exchange dead zone in the dense bed section. In addition, an axial flow gas-solid separator 41 is arranged at the end of the down-bed 32 to achieve fast and efficient gas-solid separation, reduce the burden of the subsequent filter component 44, and optimize the stable operation cycle of the entire device. By making the riser reaction component 1, the down-bed reaction component 3 and the separation circulation component 4 form a circulation pipeline, the total reaction time of the solid phase can be adjusted as needed, thereby enhancing the flexibility of operation. The gas-solid reaction device also has the advantages of saving space and large operational flexibility, and improves the reaction efficiency and system reliability as a whole.

[0038] In the embodiment of the present invention, the designer can adjust the specific structure of the axial flow gas-solid separator 41 according to the use requirements, and no specific restrictions are made here. Preferably, the axial flow gas-solid separator 41 is arranged at the end of the down-going bed 32, and the axial flow gas-solid separator 41 includes at least two forms: one is composed of structures such as guide blades, cone sections, and risers; the other is composed of a swirl head outlet. The down-going bed 32 is connected to the axial flow gas-solid separator 41 through the second reduction structure 33, and the axial flow gas-solid separator 41 is connected to the storage companion bed 43 through the separation pipeline 42. Among them, the separation pipeline 42 is composed of a purified gas discharge pipe 421 and a captured particle discharge pipe 422.

[0039] In this embodiment, the multiphase fluid reaching the end of the down-flow bed 32 is quickly separated under the combined action of inertial separation and centrifugal separation of the axial flow gas-solid separator 41. Compared with the traditional cyclone separator, the axial flow gas-solid separator 41 has a higher particle size efficiency for particles with a particle size below 20 μm, can effectively enhance the overall separation efficiency, and reduce the burden on the subsequent gas-solid separation system.

[0040] Specifically, Figure 1 As shown, along the transport direction of the ultrafine particles in the downcomer 32, an axial flow gas-solid separator 41 is provided at the end of the downcomer 32, and the purified gas discharge pipe 421 and the captured particle discharge pipe 422 in the separation pipeline 42 are both arranged on the axial flow gas-solid separator 41, providing a circulation loop for the multiphase fluid.

[0041] In an embodiment of the present invention, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the lifting pipe section 14, and a first diameter reduction structure 13 is provided between the pre-reaction section 12 and the lifting pipe section 14; and / or, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the connecting pipeline 49, and a first diameter expansion structure 11 is provided between the pre-reaction section 12 and the connecting pipeline 49; and / or, the radial dimension of the down-going bed 32 is greater than the radial dimension of the elbow 2, and a second diameter expansion structure 31 is provided between the down-going bed 32 and the elbow 2; and / or, the radial dimension of the down-going bed 32 is greater than the radial dimension of the axial flow gas-solid separator 41, and a second diameter reduction structure 33 is provided between the down-going bed 32 and the axial flow gas-solid separator 41.

[0042] Preferably, the radial dimension of the pre-reaction section 12 is larger than the radial dimension of the lifting pipe section 14, and a first diameter reduction structure 13 is provided between the pre-reaction section 12 and the lifting pipe section 14; and, the radial dimension of the pre-reaction section 12 is larger than the radial dimension of the connecting pipeline 49, and a first diameter expansion structure 11 is provided between the pre-reaction section 12 and the connecting pipeline 49; and, the radial dimension of the down-going bed 32 is larger than the radial dimension of the elbow 2, and a second diameter expansion structure 31 is provided between the down-going bed 32 and the elbow 2; and, the radial dimension of the down-going bed 32 is larger than the radial dimension of the axial flow gas-solid separator 41, and a second diameter reduction structure 33 is provided between the down-going bed 32 and the axial flow gas-solid separator 41.

[0043] By respectively arranging the first diameter expansion structure 11 and the first diameter reduction structure 13 at both ends of the pre-reaction section 12, the pre-reaction section 12 is designed to expand in diameter, which is beneficial to reducing the gas flow velocity in the pre-reaction section 12, thereby increasing the contact time between the gas and the ultrafine particles, thereby improving the reaction efficiency.

[0044] Furthermore, by arranging a second diameter expansion structure 31 and a second diameter reduction structure 33 at both ends of the down-going bed 32, the down-going bed 32 is designed with an expansion diameter, which not only significantly reduces the agglomeration of ultrafine particles during the flow process, but also moderately increases the solid phase concentration in the down-going bed 32, further improving the gas-solid contact and mixing efficiency.

[0045] Designers can adjust the shapes and structures of the first diameter-expanding structure 11 , the first diameter-reducing structure 13 , the second diameter-expanding structure 31 , and the second diameter-reducing structure 33 according to usage requirements, and no specific limitation is made here.

[0046] Preferably, the first diameter-expanding structure 11, the first diameter-reducing structure 13, the second diameter-expanding structure 31 and the second diameter-reducing structure 33 are arranged in a substantially funnel shape. The ratio of the diameter of the upstream end to the downstream end of the first diameter-reducing structure 13 is 1.2 to 3. The ratio of the diameter of the upstream end to the downstream end of the second diameter-reducing structure 33 is 0.6 to 9.

[0047] In an embodiment of the present invention, the gas-solid reaction device also includes at least one diffusion distributor 112 arranged in the pre-reaction section 12, the outlet of the connecting pipeline 49 is connected to the diffusion distributor 112, and the diffusion distributor 112 includes an outlet surface provided with diffusion holes, and the porosity of the outlet surface is 5% to 50%.

[0048] By disposing at least one diffusion distributor 112 in the pre-reaction section 12 and connecting the outlet of the connecting pipeline 49 to the diffusion distributor 112 , the gas and ultrafine particles can be more evenly distributed when entering the pre-reaction section 12 .

[0049] In addition, the outlet surface of the diffusion distributor 112 is provided with diffusion holes with an opening rate of 5% to 50%, which helps to further optimize the gas-solid mixing effect, reduce the phenomenon of local over-concentration or over-leanness, improve the uniformity of the reactants and the reaction efficiency, thereby enhancing the uniformity of gas-solid contact and helping to improve the overall performance and stability of the gas-solid reaction device.

[0050] The designer can adjust the shape, number, size and opening ratio of the diffusion holes and the opening ratio of the outlet surface according to the use requirements, and there is no specific limitation here. For example, the opening ratio of the outlet surface is 5%, 15%, 25%, 35%, 50% or other values.

[0051] In an embodiment of the present invention, the gas-solid reaction device also includes a first ring pipe distributor 111 arranged in the pre-reaction section 12, the first ring pipe distributor 111 is horizontally arranged and placed upstream of the diffusion distributor 112; and / or, the gas-solid reaction device also includes a second ring pipe distributor 46 arranged in the storage companion bed 43, the second ring pipe distributor 46 is horizontally arranged and placed at the bottom of the storage companion bed 43.

[0052] Preferably, the gas-solid reaction device comprises a first annular pipe distributor 111 disposed in the pre-reaction section 12 and a second annular pipe distributor 46 disposed in the storage companion bed 43. The second annular pipe distributor 46 in the storage companion bed 43 is lower than the captured particle discharge pipe 422 as a whole.

[0053] By setting the first ring tube distributor 111 in the pre-reaction section 12 and arranging it horizontally upstream of the diffusion distributor 112, the initial distribution of gas and ultrafine particles can be further optimized, ensuring that they have been preliminarily and evenly mixed before entering the diffusion distributor 112, thereby helping to improve the gas-solid contact efficiency and reaction uniformity in the subsequent reaction process.

[0054] Furthermore, by providing a second annular pipe distributor 46 in the storage companion bed 43 and arranging it horizontally at the bottom of the storage companion bed 43, the material distribution in the storage companion bed 43 can be effectively improved, and the occurrence of local accumulation or dead zones can be prevented, thereby improving the operating stability and reaction efficiency of the entire device.

[0055] In an embodiment of the present invention, the ratio of the diameter D1 of the pre-reaction section 12 to the diameter D2 of the riser section 14 is 1.2 to 3; and / or the bending radius R of the elbow 2 and the diameter of the elbow 2 are 0.5 to 10; and / or the ratio of the diameter D3 of the downcomer 32 to the diameter D1 of the pre-reaction section 12 is 0.5 to 3.

[0056] Preferably, the ratio of the diameter D1 of the pre-reaction section 12 to the diameter D2 of the riser section 14 is 1.2 to 3; and the bending radius R of the elbow 2 and the diameter of the elbow 2 are 0.5 to 10; and the ratio of the diameter D3 of the downcomer 32 to the diameter D1 of the pre-reaction section 12 is 0.5 to 3.

[0057] By setting the diameter D1 of the pre-reaction section 12 to 1.2 to 3 times the diameter D2 of the riser section 14, and setting the diameter D3 of the downer 32 to 0.5 to 3 times the diameter D1 of the pre-reaction section 12, the gas-solid mixing and flow characteristics can be optimized and the reaction efficiency can be improved. The diameter D2 of the riser section 14 can be the same or substantially the same as the diameter of the elbow 2.

[0058] In addition, the ratio of the bending radius R of the curved pipe 2 to the diameter of the curved pipe 2 is between 0.5 and 10. This design can effectively reduce the pressure drop in the curved pipe 2 area, reduce energy loss, ensure that gas and ultrafine particles pass through the curved pipe 2 more smoothly, and avoid problems such as increased flow resistance and particle deposition caused by excessive curvature of the curved pipe 2. Designers can adjust the specific diameter ratio according to usage needs, and no specific numerical limit is imposed here.

[0059] In an embodiment of the present invention, along the circumference of the pre-reaction section 12, at least one row of first gas-phase feed hole groups 120 are provided on the pre-reaction section 12; and / or, along the circumference of the lifting pipe section 14, at least one row of second gas-phase feed hole groups 140 are provided on the lifting pipe section 14; and / or, along the circumference of the downcomer 32, at least one row of third gas-phase feed hole groups 320 are provided on the downcomer 32.

[0060] Preferably, the pre-reaction section 12 is provided with at least one row of first gas-phase feed hole groups 120, the riser section 14 is provided with at least one row of second gas-phase feed hole groups 140, and the downer 32 is provided with at least one row of third gas-phase feed hole groups 320. The arrangement direction of the row is the height direction.

[0061] More preferably, the pre-reaction section 12 is provided with a plurality of rows of first gas-phase feed hole groups 120 , the riser section 14 is provided with a plurality of rows of second gas-phase feed hole groups 140 , and the downcomer 32 is provided with a plurality of rows of third gas-phase feed hole groups 320 .

[0062] For example, the first gas-phase feed hole group 120 is provided with 1 to 16 columns, the second gas-phase feed hole group 140 is provided with 1 to 16 columns, and the third gas-phase feed hole group 320 is provided with 1 to 16 columns.

[0063] In the embodiment of the present invention, the designer may adjust the specific structure, setting quantity and arrangement position of the first gas-phase feed hole group 120 according to the use requirements, and no specific limitation is made here.

[0064] Preferably, the first gas-phase feed hole group 120 includes at least one first gas-phase feed hole arranged on the pre-reaction section 12 along the height direction, and a first gas-phase nozzle arranged on each first gas-phase feed hole 121, and the angle α between the incident direction of the first gas-phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section 12 is 10° to 170°.

[0065] More preferably, the first gas-phase feed hole group 120 includes a plurality of first gas-phase feed holes 121 arranged along the height direction on the pre-reaction section 12. For example, each column of the first gas-phase feed hole group 120 has 2 to 10 first gas-phase feed holes 121.

[0066] In the embodiment of the present invention, the designer may adjust the specific structure, number and arrangement position of the second gas-phase feed hole group 140 according to the use requirements, and no specific limitation is made here.

[0067] Preferably, the second gas-phase feed hole group 140 includes at least one second gas-phase feed hole 141 arranged on the lifting pipe section 14 along the height direction, and a second gas-phase nozzle arranged on each second gas-phase feed hole 141, and the angle between the incident direction of the second gas-phase nozzle and the movement direction of the multiphase fluid in the lifting pipe section 14 is 10° to 170°.

[0068] More preferably, the second gas-phase feed hole group 140 includes a plurality of second gas-phase feed holes 141 arranged along the height direction on the riser section 14. For example, each row of the second gas-phase feed hole group 140 has 2 to 10 second gas-phase feed holes 141.

[0069] Designers can adjust the specific structure, number and arrangement position of the third gas-phase feed hole group 320 according to usage requirements, and no specific restrictions are made here.

[0070] Preferably, the third gas-phase feed hole group 320 includes at least one third gas-phase feed hole 321 arranged on the down-bed 32 along the height direction, and a third gas-phase nozzle arranged on each third gas-phase feed hole 321, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed 32 is 10° to 170°.

[0071] More preferably, the third gas-phase feed hole group 320 includes a plurality of third gas-phase feed holes 321 arranged along the height direction on the downer 32. For example, each column of the third gas-phase feed hole group 320 has 2 to 10 third gas-phase feed holes 321.

[0072] By respectively arranging at least one row of gas-phase feed hole groups on the pre-reaction section 12, the riser section 14 and the down-bed 32, it is possible to supplement the fluidizing gas and the raw gas during the reaction process, and multi-point gas intake can be achieved through the gas-phase feed hole groups, which helps to improve the contact opportunity and mixing uniformity of the gas and ultrafine particles, and increases the operational flexibility of the raw gas feed amount in the riser reaction assembly 1 and the down-bed reaction assembly 3.

[0073] Moreover, by setting the gas phase feed hole group, the gas distribution in each area can be better controlled to ensure that the reactants are more evenly dispersed in the entire reaction device, thereby improving the reaction efficiency and product quality. In addition, multi-point gas intake can also reduce the phenomenon of local over-concentration or over-leakage, avoid the problem of incomplete reaction or increased side reactions caused by uneven gas distribution, and enhance the operational stability and overall performance of the system.

[0074] In an embodiment of the present invention, the gas-solid reaction device further comprises a dust-containing gas filtering assembly 44 disposed on the top of the storage companion bed 43 .

[0075] By arranging the dusty gas filter assembly 44 on the top of the storage bed 43, the dust and other particulate matter generated during the reaction can be effectively removed to ensure that the discharged gas is cleaner, thereby reducing pollution to the environment and improving the operational stability of the entire system, thereby preventing equipment failure or performance degradation caused by dust accumulation. In addition, clean gas emissions also help meet environmental protection requirements and improve the overall operating efficiency and sustainability of the device.

[0076] The designer can adjust the specific structure of the dust-containing gas filter assembly 44 according to the use requirements, and no specific limitation is made here. For example, the dust-containing gas filter assembly 44 is a dust removal device such as a bag filter, an electrostatic precipitator, a cyclone separator, or the dust-containing gas filter assembly 44 can also be of other structures.

[0077] In an embodiment of the present invention, the gas-solid reaction device further comprises a discharge valve 45 disposed at the bottom of the storage companion bed 43 , and a discharge valve 47 disposed at the outlet of the storage companion bed 43 .

[0078] By arranging a discharge valve 45 at the bottom of the storage companion bed 43 and a discharge valve 47 at the outlet of the storage companion bed 43, accurate control of the flow of solid materials can be achieved.

[0079] The discharge valve 45 is located at the bottom of the storage bed 43, which helps to discharge the solid materials accumulated in the gas-solid reaction device regularly or as needed, ensuring that the operation efficiency of the gas-solid reaction device will not be affected by the accumulation of materials in the storage bed 43.

[0080] The discharge valve 47 can control the flow of materials from the storage bed 43 to the subsequent processing steps to ensure the continuity and stability of material transportation. The designer can adjust the specific models of the discharge valve 45 and the discharge valve 47 according to the use requirements, and no specific restrictions are made here.

[0081] Implementation Method 2

[0082] A gas-solid reaction method is provided in an embodiment of the present invention. The gas-solid reaction method is implemented by using the gas-solid reaction device in the first embodiment. The gas-solid reaction method comprises the following steps:

[0083] Step S1000: close the discharge valve 45, and start the gas phase supply of the second annular pipe distributor 46, so that the ultrafine particles in the storage bed 43 are in a flowing state;

[0084] Step S2000: Open the feed valve 47, and at the same time open the fluidizing gas inlet 48 to introduce fluidizing gas and feed gas into the connecting pipeline 49 to transport ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly 1 within the entrained gas range;

[0085] Step S3000: Open the first annular distributor 111 to introduce supplementary fluidizing gas into the pre-reaction section 12 to avoid the formation of a flow dead zone at the bottom of the pre-reaction section 12;

[0086] Step S4000: During the reaction of the ultrafine particles, fluidizing gas and raw material gas are introduced into the riser reaction assembly 1 and / or the downer reaction assembly 3 to maintain the raw material gas concentration in the reaction assembly; wherein the raw material gas incident speed in the riser reaction assembly 1 and / or the downer reaction assembly 3 is 10 m / s to 100 m / s;

[0087] Step S5000: After the ultrafine particles react in the riser reaction assembly 1 and the downer reaction assembly 3 in sequence, the multiphase fluid output from the downer 32 is separated by the axial flow gas-solid separator 41, and the separated ultrafine particles are transported back to the storage companion bed 43 to continue to participate in the circulation, and the separated gas phase fluid is transported back to the storage companion bed 43 and discharged after being filtered;

[0088] Step S6000: When the ultrafine particles complete the reaction cycle, the unloading valve 47 is closed to stop the cycle, and the unloading valve 45 is opened to unload the ultrafine particles.

[0089] The gas-solid reaction method of the present invention adjusts the gas phase flow rate of the fluidizing gas inlet 48 to keep the apparent gas velocity in the riser reaction assembly 1 within the entrainment gas velocity range. At the same time, the raw gas is supplemented by the gas phase nozzles provided in the riser reaction assembly 1 and the downer reaction assembly 3 to keep the raw gas in the reaction assembly always within the ideal concentration range. In addition, the axial flow gas-solid separator 41 is used to achieve efficient gas-solid separation of the multiphase fluid that completes the circulation process. In addition, the circulation or extraction of ultrafine particles is controlled by the feed valve 47 and the discharge valve 45 to achieve flexible operation of the target product production process.

[0090] Furthermore, when the ultrafine particles complete a circulation process, the axial flow gas-solid separator 41 removes most of the ultrafine particles in the multiphase fluid, and leads the ultrafine particles back to the storage companion bed 43 through the particle collection discharge pipe 422; the gas phase fluid carrying a small amount of unseparated particles will be led back to the middle of the storage companion bed 43 through the purified gas discharge pipe 421; the gas phase in the storage companion bed 43 needs to be further separated by the dust-containing gas filter assembly 44 before being discharged, and the filter element of the dust-containing gas filter assembly 44 is back-blown regularly. The ultrafine particles returned to the storage companion bed 43 will continue to participate in the circulation.

[0091] In this embodiment, the raw material gas is a gas-solid high-efficiency reaction gas, and the fluidizing gas is a protective gas such as an inert gas, which is not limited in the present invention.

[0092] In this embodiment, when a gas-solid rapid reaction is carried out in the riser reaction assembly 1 and the down-bed reaction assembly 3, the ratio of the raw gas and the fluidizing gas entering the reaction assembly through the gas phase nozzle is higher than the ratio of the raw gas and the fluidizing gas introduced through the fluidizing gas inlet 48, so as to ensure that the raw gas concentration in the reaction assembly is maintained at an ideal level.

[0093] In an embodiment of the present invention, by providing a pre-reaction section 12 with a diameter ratio of 1.2 to 3, a riser section 14 and a downer 32 with a diameter of 0.5 to 3 times the diameter D1 of the pre-reaction section 12, it is convenient to automatically adjust the superficial gas velocity in the riser reaction assembly 1 and the downer reaction assembly 3, thereby realizing the circulation and transportation of ultrafine particles in the reaction assembly.

[0094] In an embodiment of the present invention, the separated gas phase fluid is transported back to the storage companion bed 43 and discharged after filtering, which specifically includes the following steps:

[0095] Step S5100: remove a small amount of solid phase entrained in the gas phase fluid through the dusty gas filter assembly 44 and discharge the gas filtered by the dusty gas filter assembly 44. During the use of the dusty gas filter assembly 44, the dusty gas filter assembly 44 can be backwashed regularly.

[0096] In an embodiment of the present invention, the steps of introducing fluidizing gas and raw material gas into the riser reaction assembly 1 and / or the downer reaction assembly 3 to maintain the raw material gas concentration in the reaction assembly specifically include the following steps:

[0097] Step S4100: Fluidizing gas and raw gas are introduced into the pre-reaction section 12 through the first gas-phase feed hole group 120 to maintain the raw gas concentration in the reaction component; and / or, fluidizing gas and raw gas are introduced into the lifting pipe section 14 through the second gas-phase feed hole group 140 to maintain the raw gas concentration in the reaction component; and / or, fluidizing gas and raw gas are introduced into the downward bed 32 through the third gas-phase feed hole group 320 to maintain the raw gas concentration in the reaction component.

[0098] Designers can adjust the opening and closing states of each first gas-phase feed hole group 120 , each second gas-phase feed hole group 140 , and each third gas-phase feed hole group 320 according to usage requirements, and no specific limitation is made here.

[0099] All articles and references disclosed, including patent applications and publications, are incorporated herein by reference for various purposes. The term "consisting essentially of ... " describing a combination should include determined elements, ingredients, parts or steps and other elements, ingredients, parts or steps that do not substantially affect the basic novel features of the combination. The use of the terms "comprising" or "including" to describe the combination of elements, ingredients, parts or steps here also contemplates the implementation method consisting essentially of these elements, ingredients, parts or steps. Here, by using the term "may", it is intended to illustrate that any attribute described that "may" includes is optional. Multiple elements, ingredients, parts or steps can be provided by a single integrated element, ingredient, part or step. Alternatively, a single integrated element, ingredient, part or step can be divided into separate multiple elements, ingredients, parts or steps. The disclosure "one" or "one" used to describe an element, ingredient, part or step is not said to exclude other elements, ingredients, parts or steps.

[0100] Each embodiment in this specification is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same and similar parts between the embodiments can be referred to each other. The above embodiments are only for illustrating the technical concept and features of the present invention. The purpose is to enable people familiar with this technology to understand the content of the present invention and implement it accordingly, and it cannot be used to limit the scope of protection of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A gas-solid reaction device, characterized in that: include: A riser reaction assembly, the riser reaction assembly comprising a pre-reaction section and a riser section connected to an outlet of the pre-reaction section; A downer bed reaction assembly, the downer bed reaction assembly comprises a downer bed, the downer bed and the riser pipe section are arranged side by side, and the inlet of the downer bed is connected with the outlet of the riser pipe through a bend pipe; A separation circulation component, the separation circulation component comprises an axial flow gas-solid separator, a storage companion bed, and a connecting pipeline connecting the outlet of the storage companion bed and the inlet of the pre-reaction section, the connecting pipeline is provided with a fluidizing gas inlet, the inlet of the axial flow gas-solid separator is connected to the outlet of the descending bed, the gas phase outlet of the axial flow gas-solid separator is connected to the gas phase area of ​​the storage companion bed through a purified gas discharge pipe, and the solid phase outlet of the axial flow gas-solid separator is connected to the storage area of ​​the storage companion bed through a captured particle discharge pipe.

2. The gas-solid reaction device according to claim 1, characterized in that: The radial dimension of the pre-reaction section is larger than the radial dimension of the lifting pipe section, and a first diameter reduction structure is provided between the pre-reaction section and the lifting pipe section; and / or, the radial dimension of the pre-reaction section is larger than the radial dimension of the connecting pipeline, and a first diameter expansion structure is provided between the pre-reaction section and the connecting pipeline; and / or, the radial dimension of the down-going bed is larger than the radial dimension of the elbow, and a second diameter expansion structure is provided between the down-going bed and the elbow; and / or, the radial dimension of the down-going bed is larger than the radial dimension of the axial flow gas-solid separator, and a second diameter reduction structure is provided between the down-going bed and the axial flow gas-solid separator.

3. The gas-solid reaction device according to claim 1, characterized in that: The gas-solid reaction device also includes at least one diffusion distributor arranged in the pre-reaction section, the outlet of the connecting pipeline is connected to the diffusion distributor, and the diffusion distributor includes an outlet surface provided with diffusion holes, and the opening rate of the outlet surface is 5% to 50%.

4. The gas-solid reaction device according to claim 3, characterized in that: The gas-solid reaction device also includes a first ring pipe distributor arranged in the pre-reaction section, the first ring pipe distributor is horizontally arranged and placed upstream of the diffusion distributor; and / or, the gas-solid reaction device also includes a second ring pipe distributor arranged in the material storage companion bed, the second ring pipe distributor is horizontally arranged and placed at the bottom of the material storage companion bed.

5. The gas-solid reaction device according to claim 4, characterized in that: The ratio of the diameter of the pre-reaction section to the diameter of the riser section is 1.2 to 3; and / or the bending radius R of the elbow and the diameter of the elbow are 0.5 to 10; and / or the ratio of the diameter of the downcomer to the diameter of the pre-reaction section is 0.5 to 3.

6. The gas-solid reaction device according to claim 5, characterized in that: Along the circumference of the pre-reaction section, at least one row of first gas-phase feed hole groups are provided on the pre-reaction section; and / or, along the circumference of the riser section, at least one row of second gas-phase feed hole groups are provided on the riser section; and / or, along the circumference of the downer, at least one row of third gas-phase feed hole groups are provided on the downer.

7. The gas-solid reaction device according to claim 6, characterized in that: The first gas-phase feed hole group includes at least one first gas-phase feed hole arranged on the pre-reaction section along the height direction, and a first gas-phase nozzle arranged on each of the first gas-phase feed holes, and the angle between the incident direction of the first gas-phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section is 10° to 170°; and / or, the second gas-phase feed hole group includes at least one second gas-phase feed hole arranged on the riser section along the height direction, and a second gas-phase nozzle arranged on each of the second gas-phase feed holes, and the angle between the incident direction of the second gas-phase nozzle and the movement direction of the multiphase fluid in the riser section is 10° to 170°; and / or, the third gas-phase feed hole group includes at least one third gas-phase feed hole arranged on the down-bed along the height direction, and a third gas-phase nozzle arranged on each of the third gas-phase feed holes, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed is 10° to 170°.

8. The gas-solid reaction device according to claim 6, characterized in that: The gas-solid reaction device also includes a dust-containing gas filtering assembly arranged on the top of the material storage companion bed.

9. The gas-solid reaction device according to claim 8, characterized in that: The gas-solid reaction device further comprises a discharge valve arranged at the bottom of the material storage companion bed, and a feed discharge valve arranged at the outlet of the material storage companion bed.

10. A gas-solid reaction method, characterized in that: The gas-solid reaction method is implemented by using the gas-solid reaction device as claimed in claim 9, and comprises the following steps: Close the discharge valve and start the gas phase supply of the second ring pipe distributor to make the ultrafine particles in the storage bed flow; Open the feed valve and the fluidizing gas inlet at the same time to introduce fluidizing gas and feed gas into the connecting pipeline to transport ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly within the entrained gas range; Opening the first annular distributor to introduce supplementary fluidizing gas into the pre-reaction section to avoid formation of a flow dead zone at the bottom of the pre-reaction section; During the reaction of the ultrafine particles, fluidizing gas and raw material gas are introduced into the riser reaction assembly and / or the downer reaction assembly to maintain the raw material gas concentration in the reaction assembly; wherein the raw material gas injection velocity in the riser reaction assembly and / or the downer reaction assembly is 10 m / s to 100 m / s; After the ultrafine particles have reacted in the riser reaction assembly and the downer reaction assembly in sequence, the multiphase fluid output from the downer is separated by an axial flow gas-solid separator, the separated ultrafine particles are transported back to the storage companion bed to continue to participate in the circulation, and the separated gas phase fluid is transported back to the storage companion bed and discharged after being filtered; When the ultrafine particles complete the reaction cycle, the feed valve is closed to stop the cycle, and the discharge valve is opened to discharge the ultrafine particles.

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