Circulating fluidized reactor system and method of use

Abstract

The application discloses a circulating fluid reactor system and a use method, and belongs to the field of chemical production equipment. The system comprises a circulating fluid reaction cylinder which is provided with a material port and a reaction cavity; material entering from the material port and the lower end is reacted in the reaction cavity and then discharged from the upper end; the material flows in the reaction cavity from the lower end to the upper end; a feeding dispersion device is connected to the lower end; a reaction heat removal device is used for heat exchange with fluid in the reaction cavity and provides a cold source; a separation device is in communication with the upper end and is provided with a first outlet and a second outlet; a material circulation device is connected to the second outlet at one end and connected to the feeding dispersion device at the other end; the use method comprises the following steps: starting the reaction heat removal device, and feeding material; adjusting the temperature through the reaction heat removal device; maintaining the pressure in the reaction cavity and the material flow rate; and regenerating and refluxing through the material circulation device. The application can strengthen the mass transfer and heat transfer of the reaction, effectively eliminate hot spot effect, and improve production effect and efficiency.

Description

Technical Field

[0001] This application belongs to the field of chemical production equipment technology, and in particular relates to a circulating fluidized reactor system and its usage method. Background Technology

[0002] Propylene oxide (PO) is an important propylene derivative, mainly used in the production of polyether polyols, propylene glycol, propylene carbonate, and other products, with wide applications in the petroleum, chemical, pesticide, textile, and daily chemical industries. Propylene oxide can be prepared through methods such as direct oxidation with hydrogen peroxide, co-oxidation, and chlorohydrin methods. The direct redox reaction between hydrogen peroxide and propylene to produce propylene oxide is a simple process with mild reaction conditions, making it environmentally friendly and one of the fastest-growing and most promising technologies currently available.

[0003] The direct oxidation of propylene with hydrogen peroxide to produce propylene oxide is a strongly exothermic reaction. The heat of reaction needs to be removed in time; otherwise, the local temperature in the system will become too high, leading to the self-decomposition of hydrogen peroxide and other side reactions, which will reduce the effective utilization rate of hydrogen peroxide and the selectivity of the target product.

[0004] Currently, industrial plants typically use tubular fixed-bed reactors for propylene oxide production. However, this type of reactor presents several problems in producing propylene oxide. The reaction is uneven across different parts of the bed, making it prone to short circuits, localized hot spots, and side reactions. The effective utilization rate of hydrogen peroxide and the selectivity for propylene oxide are also low. Furthermore, the catalyst lifespan is shortened, requiring catalyst regeneration every one to two months, which severely impacts the plant's operating cycle and the company's economic benefits. For reactions prone to localized hot spots, timely deheating is crucial, and currently, there is no suitable chemical production plant for this purpose. Summary of the Invention

[0005] This application aims to solve, at least to some extent, the technical problem of local hot spots easily generated in chemical production equipment. To this end, this application provides a circulating fluidized reactor system and its usage method, which can effectively eliminate internal diffusion resistance, fully utilize the efficiency of reactants and catalysts, enhance the mass and heat transfer of the reaction, and enable reactants and catalysts to have good dispersibility, activity and selectivity, thereby eliminating the hot spot effect in the equipment, reducing the generation of by-products and extending the catalyst cycle.

[0006] In a first aspect, embodiments of this application provide a circulating fluidized reactor system, comprising:

[0007] A circulating fluidized bed reactor has a lower end for feeding and an upper end for discharging, with the upper end higher than the lower end. A material inlet is located on the side of the reactor for feeding. Inside the reactor is a reaction chamber connecting the upper end, the lower end, and the material inlet, providing space for the reaction. Material entering the reaction chamber through the material inlet reacts with material entering the reaction chamber through the lower end, and is then discharged through the upper end. The material flows in a fluid form after entering and reacting within the reaction chamber, and the flow direction is consistent with the flow direction from the lower end to the upper end.

[0008] The feeding and dispersing device is connected to the lower end. The feeding and dispersing device is used to disperse the material and inject the dispersed material into the reaction chamber through the lower end.

[0009] The reaction heat dissipation device is partly located in the reaction chamber for heat exchange with the fluid in the reaction chamber; the other part is located outside the circulating fluidized reaction cylinder to provide a cold source.

[0010] A separation device is used to separate products. The separation device is connected to the upper end and has a first outlet for separating products and a second outlet for separating residues.

[0011] The material circulation device is used to regenerate the separated residue and circulate it back to the feeding dispersion device. One end of the material circulation device is connected to the second outlet, and the other end is connected to the feeding dispersion device.

[0012] In an optional embodiment, the feeding and dispersing device includes a variable diameter section and a mixing section. The mixing section is connected to the lower end and is connected to the material circulation device. One end of the variable diameter section is provided with an end feed port, and the opposite end of the variable diameter section is connected to the mixing section. The variable diameter section has a fluid channel that runs through both ends. The diameter of the middle part of the fluid channel is smaller than the diameter of the two ends, and the diameter of the fluid channel gradually changes from one end to the other end. The variable diameter section is also provided with a lateral feed port, which is connected to the variable diameter position of the fluid channel near the mixing section. Multiple lateral feed ports are provided.

[0013] In an optional embodiment, the mixing section includes a mixing member and a baffle. The mixing member is connected to the variable diameter section. The mixing member has multiple holes for dispersing materials. The baffle is located on the top of the mixing member and blocks the holes located on the top of the mixing member to prevent clogging of the holes.

[0014] In an optional embodiment, the circulating fluidized bed reactor is divided into multiple sections from the bottom to the top. Each section of the circulating fluidized bed reactor is provided with a material inlet. The section closer to the bottom is called the lower section reactor reactor, and the section closer to the top is called the upper section reactor reactor. The length of the lower section reactor reactor is shorter than that of the upper section reactor reactor.

[0015] In an optional embodiment, a segmented feeding device is also included, comprising multiple segmented feeding pipes and multiple feeding distribution components. The segmented feeding pipes are respectively connected to each material inlet, and the segmented feeding pipes are correspondingly connected to the feeding distribution components. The feeding distribution components are located inside the reaction chamber. Through the multiple segmented feeding pipes, materials can be injected into a multi-segment circulating fluidized reaction cylinder.

[0016] In an optional embodiment, the reaction heat removal device includes a cold source pressurization component, a cooling component, a cold source inlet pipe, a cold source outlet pipe, and a heat exchanger. The heat exchanger is located inside the reaction chamber. The cold source inlet pipe is connected to the inlet of the heat exchanger, and the cold source outlet pipe is connected to the outlet of the heat exchanger, so that the cold source flow direction in the heat exchanger is opposite to the direction from the top to the bottom. The cold source inlet pipe is connected to the cooling component, and the cold source outlet pipe is connected to the cold source pressurization component. The cold source pressurization component is connected to the cooling component. The cold source pressurization component is used to pressurize the cold source, and the cooling component is used to cool the cold source.

[0017] In an alternative embodiment, the material circulation device includes components with progressively decreasing heights:

[0018] A buffer assembly is used to buffer the material. The buffer assembly is lower than the separation device and is connected to the second outlet. The bottom of the buffer assembly is provided with a discharge pipe for discharging the separation residue.

[0019] The regeneration component is used to regenerate the separated residue. The side wall of the regeneration component is provided with a high-temperature regeneration liquid inlet, a regeneration liquid outlet and a low-temperature regeneration liquid inlet with decreasing heights. The top of the regeneration component is connected to the buffer component.

[0020] The pressure barrier assembly is used to allow the separated residue to pass through and to block it in order to maintain the pressure difference. The top of the pressure barrier assembly is connected to the buffer assembly and the regeneration assembly respectively. The top of the pressure barrier assembly is also provided with a feeding section for replenishing materials. The bottom of the pressure barrier assembly is connected to the mixing section.

[0021] Secondly, embodiments of this application provide a method for using a circulating fluidized bed reactor system, which employs the aforementioned circulating fluidized bed reactor system. The method of use includes:

[0022] Start the reaction cooling device and introduce materials into the circulating fluidized reaction cylinder through the feeding dispersion device and the material inlet respectively;

[0023] The temperature in the reaction chamber is adjusted by a reaction cooling device to maintain the temperature in the reaction chamber at [20℃, 60℃].

[0024] Material is injected into the reaction chamber through a feeding and dispersing device and through a material inlet, so that the pressure range in the reaction chamber is [1.6 MPa, 3.5 MPa] and the apparent flow rate of the material in the reaction chamber is [0.02 m / s, 0.5 m / s].

[0025] The reaction products and residues are separated by a separation device, and the residues are then regenerated and returned to the feed dispersion device by a material circulation device.

[0026] In an optional embodiment, when the circulating fluidized reaction cylinder is provided with multiple sections, the temperature of the cold source in the reaction heat removal device corresponding to the lower section of the reaction cylinder is lower than the temperature of the cold source in the reaction heat removal device corresponding to the upper section of the reaction cylinder.

[0027] In an optional embodiment, in the material circulation device, the temperature of the regenerated liquid introduced into the high-temperature regenerated liquid inlet is [100℃, 150℃], the temperature of the regenerated liquid introduced into the low-temperature regenerated liquid inlet is [20℃, 60℃], and the pressure inside the regeneration component is [2.0Mpa, 3.5Mpa].

[0028] As can be seen from the above technical solution, the beneficial effects of this application are as follows:

[0029] 1. The system of this application changes the existing fixed contact reaction production method. By using a feeding dispersion device to fully disperse the material and mix it thoroughly with the material returning from the material circulation device, the material enters the reaction chamber and reacts with the material entering through the material inlet. The material always flows from the bottom to the top in the reaction chamber. In this way, the material reacts while flowing in the circulating fluidized reaction cylinder. The heat generated by the reaction is then quickly transferred away by the reaction heat removal device. This flow reaction and heat exchange ensures that there is no heat stagnation in the entire reaction chamber, thus preventing the generation of local hot spots. The product is then separated from the top by a separation device. The unseparated material is regenerated and replenished by the material circulation device and returned to the feeding dispersion device to enter the next cycle. Since the materials in chemical production include reactants and catalysts, the above method can effectively eliminate internal diffusion resistance, fully utilize the efficiency of reactants and catalysts, enhance the mass and heat transfer of the reaction, and give reactants and catalysts good dispersibility, activity, and selectivity. This eliminates the hot spot effect in the device, reduces the generation of by-products, and extends the catalyst cycle.

[0030] 2. The method of use described in this application involves adding material through a feeding and dispersing device and a material inlet, maintaining the pressure in the reaction chamber within a certain range and ensuring a certain flow rate of the material. This facilitates material dispersion and contact, allowing the material to react fully within the reaction chamber without generating localized hot spots. Simultaneously, by maintaining the temperature of the reaction chamber within a certain range, side reactions are less likely to occur, and heat can be removed in a timely manner. This promotes the formation of reaction products, reduces other products, and thus improves production efficiency and effectiveness. It also effectively utilizes reactants and catalysts, enabling the production equipment to operate efficiently and stably. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are some embodiments of this application. For those skilled in the art, other embodiments and drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 A schematic diagram illustrating an embodiment of the circulating fluidized reactor system and its usage method of the present invention is shown;

[0033] Figure 2 A schematic diagram illustrating the steps of an embodiment of the circulating fluidized reactor system and its usage method of the present invention is shown;

[0034] Reference numerals: 100, reactor system; 110, feed dispersion device; 111, variable diameter section; 111a, fluid channel; 111b, end feed inlet; 111c, side feed inlet; 112, mixing section; 113, mixing component; 114, baffle; 120, circulating fluidized bed reactor; 120a, material inlet; 121, lower end; 122, upper end; 123, reaction chamber; 124, lower section reactor; 125, upper section reactor; 130, reaction heat removal device; 131, cold source pressurization assembly; 132, cooling assembly; 133 134. Cold source inlet pipe; 135. Cold source outlet pipe; 140. Heat exchanger; 141. Segmented feeding device; 142. Segmented feeding pipe; 143. Feed distribution device; 150. Separation device; 151. First outlet; 152. Second outlet; 160. Material circulation device; 161. Buffer assembly; 161a. Discharge pipe; 162. Regeneration assembly; 162a. High-temperature regenerated liquid inlet; 162b. Low-temperature regenerated liquid inlet; 162c. Regenerated liquid outlet; 163. Pressure barrier assembly; 163a. ​​Feeding section; 164. Pressurization assembly. Detailed Implementation

[0035] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0036] It should be noted that all directional indications in the embodiments of the present invention are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0037] In this invention, unless otherwise explicitly specified and limited, the terms "connection," "fixed," etc., should be interpreted broadly. For example, "fixed" can mean a fixed connection, a detachable connection, or an integral part; it can mean a mechanical connection or an electrical connection; it can mean a direct connection or an indirect connection through an intermediate medium; it can mean the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0038] Furthermore, in this invention, descriptions involving "first," "second," etc., are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of that feature. Additionally, the technical solutions of the various embodiments can be combined with each other, but only on the basis of being achievable by those skilled in the art. When the combination of technical solutions is contradictory or impossible to implement, such a combination of technical solutions should be considered non-existent and not within the scope of protection claimed by this invention.

[0039] This application is described below with reference to the accompanying drawings and specific embodiments:

[0040] Please refer to Figure 1The first aspect of this application provides a circulating fluidized bed reactor system, which includes a circulating fluidized bed reactor 120, a feed dispersion device 110, a reaction heat removal device 130, a separation device 150, and a material circulation device 160. The materials include reactants and a catalyst, and the catalyst can flow in the material circulation device 160. The circulating fluidized bed reactor 120 has a lower end 121 for feeding and an upper end 122 for discharging. The upper end 122 is higher than the lower end 121. The circulating fluidized bed reactor 120 is a cylindrical structure and is vertically arranged. The lower end 121 is the bottom of the cylindrical structure and the upper end 122 is the top of the cylindrical structure. The side of the circulating fluidized bed reactor 120 is provided with a material inlet 120a for feeding, so the material has two inlets, namely the lower end 121 and the material inlet 120a. The circulating fluidized bed reactor 120 is provided with a reaction chamber 123 that connects the upper end 122, the lower end 121, and the material inlet 120a. The body structure is in the form of a shell with an internal cavity. The reaction chamber 123 is used to provide space for material reaction. Material entering the reaction chamber 123 through the material inlet 120a reacts with material entering the reaction chamber 123 through the lower end 121. After the reaction, the material is discharged from the circulating fluidized reaction cylinder 120 through the upper end 122. After entering the reaction chamber 123, the material flows in the form of fluid after the reaction. That is, the material starts to flow as soon as it enters, and reacts while flowing. The products and residues obtained from the reaction also flow along with it, and the flow direction is consistent with the flow direction from the lower end 121 to the upper end 122, such as flowing from bottom to top.

[0041] A feeding and dispersing device 110 is connected to the lower end 121. The feeding and dispersing device 110 has an inlet and an outlet. The inlet is for material to enter, and the outlet is for connecting to the lower end 121 and discharging the material. The feeding and dispersing device 110 disperses the material and injects the dispersed material into the reaction chamber 123 through the lower end 121. The feeding and dispersing device 110 can adopt various structural forms, such as a Venturi tube or an atomizing device, as long as it can disperse the material into small particles. A reaction cooling device 130 is partially located in the reaction chamber 123. In section 23, a heat exchange mechanism is used for heat exchange with the fluid in reaction chamber 123. This mechanism, such as heat exchange plates or tubes, is located within reaction chamber 123. Another section is located outside the circulating fluidized bed reactor 120 to provide a cooling source. This can be achieved by using a cooling pump connected to a pipeline, which is connected to the heat exchange mechanism. The cooling source can also be a liquid cooling source. A separation device 150 is used to separate the products. This device is connected to the upper section 122, and the products and residues are separated from the circulating fluidized bed reactor 120. After exiting from 20, the residue enters the separation device 150 for separation. The separation device 150 can be a centrifugal separator, liquid-solid separator, etc. The separation device 150 is provided with a first outlet 151 for separating the product and a second outlet 152 for separating the residue. The first outlet 151 is located at the top of the separation device 150, and the second outlet 152 is located at the bottom of the separation device 150. The lighter product is separated out through the first outlet 151, and the heavier residue is discharged through the second outlet 152. The material circulation device 160 is used to regenerate the separated residue and circulate it back to the feeding dispersion device 110. One end of the material circulation device 160 is connected to the second outlet 152, and the other end is connected to the feeding dispersion device 110. The material circulation device 160 can be a pipeline with a one-way valve, and a residue regeneration device is set on the pipeline. The regeneration device is like a catalyst regenerator. The residue is the catalyst after the reaction. The catalyst enters the regenerator to restore the catalytic effect and eliminate the failed part of the catalyst. Then it is circulated back to the feeding dispersion device 110 for the next cycle.

[0042] Existing chemical production equipment cannot effectively eliminate localized hot spots. For example, the tubular fixed-bed reactor commonly used in propylene oxide production, while able to transfer heat generated during the reaction to some extent, suffers from poor heat and mass transfer between reactants and products due to its working principle. This easily leads to localized hot spots in the reaction zone, resulting in numerous side reactions and severely impacting production efficiency and subsequent product purification processes. It also causes problems such as short catalyst cycles. This application changes the existing fixed-contact reaction production method by using a feed dispersion device 110 to fully disperse the material and mix it thoroughly with the material returning from the material circulation device 160 before entering the reaction chamber 123. There, the material reacts with the material entering through the material inlet 120a. The material in the reaction chamber 123 always flows from the lower end 121 to the upper end 122. This allows the material to react while flowing in the circulating fluidized reaction cylinder 120, and the heat generated during the reaction is quickly transferred away by the reaction heat removal device 130. This flow reaction and heat exchange ensures that there is no heat stagnation in the entire reaction chamber 123, thus preventing... Local hot spots are generated, and the product is then separated from the upper end 122 by the separation device 150. The unseparated material is then regenerated and replenished by the material circulation device 160 and returned to the feed dispersion device 110 to enter the next cycle. Since the materials in chemical production include reactants and catalysts, the above method can effectively eliminate internal diffusion resistance, fully utilize the efficiency of reactants and catalysts, enhance the mass and heat transfer of the reaction, and give reactants and catalysts good dispersibility, activity and selectivity, thereby eliminating the hot spot effect in the device, reducing the generation of by-products and extending the catalyst cycle.

[0043] Please refer to Figure 2 In an optional embodiment, the feeding and dispersing device 110 includes a variable diameter section 111 and a mixing section 112. The top end of the mixing section 112 is connected to the lower end 121. The mixing section 112 is connected to the material circulation device 160, and one end of the material circulation device 160 is connected to the side of the mixing section 112. One end of the variable diameter section 111 is provided with an end feed port 111b, and the opposite end of the variable diameter section 111 is connected to the mixing section 112. The mixing section 112 and the variable diameter section 111 are connected vertically. The variable diameter section 111 has a fluid channel 111a that extends through both ends. The middle diameter of the fluid channel 111a is smaller than that of the lower end. The fluid channel 111a has two diameters, and the diameter of the fluid channel 111a gradually changes from one end to the other. For example, the diameter-changing part 111 adopts a micron-sized porous Venturi tube. Methanol is used as the material and is injected upward into the Venturi tube from the end inlet 111b. The diameter-changing part 111 is also provided with a side inlet 111c. The side inlet 111c is connected to the diameter-changing position of the fluid channel 111a near the mixing part 112. Propylene enters the Venturi tube through the side inlet 111c. There are multiple side inlets 111c. Multiple side inlets 111c can be opened along the side of the Venturi tube, thus forming multiple inlets for propylene to enter the Venturi tube.

[0044] In an optional embodiment, the mixing section 112 includes a mixing element 113 and a baffle 114. The mixing element 113 is connected to the reducing section 111, and the bottom end of the mixing element 113 is connected to the top end of the reducing section 111. Material can enter the mixing element 113 through a venturi tube. The mixing element 113 has multiple holes for dispersing the material. The mixing element 113 has a porous structure, with its top and bottom ends connected. The multiple holes facilitate dispersion of the material after it enters. Thus, the material is first dispersed through the venturi tube and then further dispersed through the mixing element 113. To fully disperse the material... The material is dispersed, and the mixing element 113 can adopt a honeycomb-like structure. The baffle 114 is located on the top of the mixing element 113. The baffle 114 blocks the holes on the top of the mixing element 113 to prevent blockage of the holes and entry into the mixing element 113. Since the catalyst uses small particles, it may fall into the holes under the action of gravity. The baffle 114 adopts a conical structure. In the longitudinal section view, the baffle 114 can form a triangular block above the holes. The edge of the baffle 114 is spaced from the top of the mixing element 113, and the material can enter the reaction chamber 123 from the gap. Specifically, when methanol enters the Venturi tube, the material flow rate increases due to the narrowing of the venturi tube throat, creating a negative pressure at the throat. This draws propylene in through the lateral feed inlet 111c on the sidewall of the Venturi tube, resulting in a violent vertical collision. The propylene is eventually dispersed into microdroplets with a diameter of 100-300 micrometers, which are then incorporated into the methanol. This increases the mass transfer area for the propylene reaction. The uniformly mixed methanol-propylene mixture disperses the recycled catalyst at the mixing unit 113, and then carries the catalyst particles uniformly upward into the reaction chamber 123.

[0045] In an optional embodiment, the circulating fluidized bed reactor 120 is divided into multiple sections from the lower end 121 to the upper end 122. The circulating fluidized bed reactor 120 is a vertical cylinder, such as being divided into 3-4 sections. Each section of the circulating fluidized bed reactor 120 is provided with a material inlet 120a, and a reaction heat dissipation device 130 is provided in the reaction chamber 123 of each section of the circulating fluidized bed reactor 120. For example, a heat exchange mechanism is bolted to the inner wall of each section of the circulating fluidized bed reactor 120. The section closer to the lower end 121 is called the lower section reactor 124, and the section closer to the upper end 122 is called the upper section reactor 125. The length of the lower section reactor 124 is less than that of the upper section reactor 125. In an optional embodiment, the top of the uppermost section of the circulating fluidized reaction cylinder 120 is connected to the side wall of the separation device 150 via a pipe. This pipe cuts into the inner wall of the separation device 150 to form a cyclone settling structure, which can improve the separation efficiency of the catalyst. The separation device 150 adopts a cylindrical structure, with a slender upper part that is conducive to increasing the residence time and ensuring the full separation of the catalyst. The lower part is conical to facilitate catalyst aggregation. The bottom is connected to the buffer assembly 161 of the material circulation device 160 via a catalyst conveying pipe.

[0046] In an optional embodiment, a segmented feeding device 140 is also included, comprising multiple segmented feeding pipes 141 and multiple feeding distributors 142. The segmented feeding pipes 141 are respectively connected to each material inlet 120a, and the segmented feeding pipes 141 are correspondingly connected to the feeding distributors 142. The feeding distributors 142 are located within the reaction chamber 123. The feeding distributors 142 utilize existing distributors. The material enters the distributor after passing through the segmented feeding pipes 141, and is then dispersed within the reaction chamber 123 by the distributor. If a hydrogen peroxide distributor is used, the distributor can be annular or tree-shaped, with nozzles evenly distributed to ensure mixing with the material. Uniform; through multiple segmented feed pipes 141, materials can be injected into multi-segment circulating fluidized reaction cylinders 120. The feed distribution component 142 is placed below and close to the heat exchange mechanism of the reaction heat removal device 130. Since the cold source in the heat exchange mechanism flows downward, the liquid in the reaction chamber 123 flows upward, which allows the fluid to fully exchange heat with the cold source and allows the fluid flowing through the heat exchange mechanism to be fully cooled. If the feed distribution component 142 is set at the bottom of each segment of the circulating fluidized reaction cylinder 120, and each segment of the circulating fluidized reaction cylinder 120 is equipped with a heat exchange mechanism, the material will flow upward and undergo heat exchange after entering.

[0047] In an optional embodiment, the reaction cooling device 130 includes a cold source pressurization assembly 131, a cooling assembly 132, a cold source inlet pipe 133, a cold source outlet pipe 134, and a heat exchanger 135, forming an independent closed-loop cooling circuit. Each component is filled with a cold source, which is chilled water. The heat exchanger 135 is located inside the reaction chamber 123 and can be a heat exchange tube. A cold source is introduced into the heat exchange tube, which can be a smooth tube, a twisted tube, a corrugated tube, or other types of pipe. The top of the heat exchanger 135 is the inlet, and the bottom is the outlet. The cold source inlet pipe 133 is connected to the inlet of the heat exchanger 135, and the cold source outlet pipe 134 is connected to the outlet of the heat exchanger 135, so that the flow direction of the cold source in the heat exchanger 135 is opposite to the direction from the upper end 122 to the lower end 121. The cold source inlet pipe 133 and the cold source outlet pipe 134 are connected in opposite directions. 34. Multiple sets of cold source inlet pipes 133 and cold source outlet pipes 134 are set up in parallel. Each set of cold source inlet pipes 133 and cold source outlet pipes 134 corresponds to each section of circulating fluidized reactor 120. For example, when there are 4 sections of circulating fluidized reactor 120, 4 sets of cold source inlet pipes 133, cold source outlet pipes 134 and heat exchange components 135 are set up respectively, numbered from bottom to top as section one to section four. Among them, the length of the heat exchange components corresponding to section one and two is set to be shorter, and the length of the heat exchange components corresponding to section three and four is set to be longer. This is conducive to quickly removing the heat of reaction, controlling the reaction temperature, and preventing the reaction from overheating. The mixture of reactants and catalysts flows upward and reacts. Since the catalyst is uniformly dispersed in the reactants, the reactants can react rapidly on the catalyst surface. The reaction products and heat of reaction can also be quickly moved into the reactants. The reaction is uniform, there is no hot spot phenomenon, and the selectivity of the reaction products is high. The cold source inlet pipe 133 is connected to the cooling component 132, which is used to cool the cold source. The cooling component 132 can be a cooler, a chilled water heat exchanger, or a closed cooling tower, depending on the requirements. The cold source outlet pipe 134 is connected to the cold source pressurization component 131, which is connected to the cooling component 132. The cold source pressurization component 131 uses a cold source circulation pump to provide pump pressure and is used to pressurize the cold source.

[0048] In an optional embodiment, the material circulation device 160 includes, in descending order of height, a buffer assembly 161, a regeneration assembly 162, and a pressure barrier assembly 163. The buffer assembly 161 is used to buffer the material. The buffer assembly 161 is lower than the separation device 150 and is connected to the second outlet 152. In this way, the catalyst particles settle to the bottom of the separation device 150 and flow into the buffer assembly 161 by gravity through the catalyst delivery pipe. The catalyst delivery pipe may be equipped with a valve. The buffer assembly 161 is a buffer hopper, which is a cylindrical container with an annular baffle inside. The lower part of the hopper is connected to a washing medium pipe. The washing medium enters the annular gap between the annular baffle and the container shell, flows upward from the bottom of the annular gap, and contacts the catalyst to wash away the reaction products carried by the catalyst. The bottom of the buffer hopper is connected to the pressure barrier assembly 163 and the regeneration assembly 162 through another catalyst delivery pipe. The catalyst delivery pipe is equipped with a discharge pipe 161a, located at the bottom of the buffer assembly 161, which can be used for online unloading operations, such as discharging residues. The discharge pipe 161a is equipped with a valve for easy opening and closing control. The pressure barrier assembly 163 is used to allow the separation residue to pass through and to block it in order to maintain the pressure difference. The pressure barrier assembly 163 adopts a closed hopper, which is a conical container. It can adjust the pressure between the regeneration assembly 162 and the circulating fluidized reaction cylinder 120, and can guide the catalyst to circulate and maintain the stable operation of the catalyst. The top of the pressure barrier assembly 163 is connected to the buffer assembly 161 and the regeneration assembly 162 respectively. The top of the pressure barrier assembly 163 is also provided with a feeding part 163a for replenishing materials. For example, the top of the closed hopper is connected to a pipe, and the top of the pipe is a funnel. The catalyst is added to the closed hopper through the funnel, which can realize the online replacement of the catalyst. The bottom of the pressure barrier assembly 163 is connected to the mixing part 112. That is, the bottom of the closed hopper is connected to the side wall of the mixing part 112 through a pipe and is connected to the hole of the mixing part 113.

[0049] In an optional embodiment, the regeneration component 162 is used to regenerate the separated residue. The top of the regeneration component 162 is connected to the buffer component 161. The catalyst enters the regeneration component 162 from the buffer component 161. The regeneration component 162 is a regenerator. In order to maintain the high activity and selectivity of the catalyst, it is necessary to regenerate the partially deactivated catalyst to restore its activity. The regenerator employs a two-stage regeneration process. Specifically, the sidewall of the regeneration component 162 is equipped with a high-temperature regenerated liquid inlet 162a, a regenerated liquid outlet 162c, and a low-temperature regenerated liquid inlet 162b, with their heights decreasing sequentially. The high-temperature regenerated liquid inlet 162a is located at the upper part of the regenerator, and the low-temperature regenerated liquid inlet 162b is located at the lower part of the regenerator. The high-temperature regenerated liquid inlet 162a, the regenerated liquid outlet 162c, and the low-temperature regenerated liquid inlet 162b are connected to external pipes. The high-temperature regenerated liquid inlet 162a is supplied with a higher-temperature regenerated liquid, which flows downward and contacts the catalyst awaiting regeneration in the forward direction, replacing most of the poisons in the catalyst. The low-temperature regenerated liquid inlet 162b is supplied with a lower-temperature regenerated liquid, which flows upward and contacts the catalyst awaiting regeneration in the reverse direction, replacing and washing away the remaining poisons, fully restoring the catalyst activity, and simultaneously lowering the catalyst temperature. Methanol is used as the regenerated liquid. After replacement, the high-temperature and low-temperature regenerated liquids merge in the middle of the regenerator and leave the regenerator through the regenerated liquid outlet 162c, which is then sent downstream for further processing and recycling. In an optional embodiment, a booster assembly 164, such as an existing elevator, can be provided to lift the material from a lower position to a higher position. The booster assembly 164 is suitable when the height of the material coming out of the pressure barrier assembly 163 is lower than the connection point with the feed dispersion device 110. The material discharged from the pressure barrier assembly 163 enters the lower position, and the booster assembly 164 is used to pressurize the material from the lower position to the connection point at the higher position and then enter the feed dispersion device 110.

[0050] In summary, taking the production of epoxy propylene as an example, the raw materials and hydrogen peroxide are fully mixed in the feeding and dispersing device 110 located at the bottom of the circulating fluidized reactor 120, and then mixed with the circulating catalyst. The catalyst is uniformly dispersed in the reactants to form a stable dispersion mixture, which then enters the reaction chamber 123 and flows upward along the circulating fluidized reactor 120. The hydrogen peroxide is dispersed by the segmented feeding device 140. The above dispersion mixture is fully mixed with the hydrogen peroxide sprayed by the hydrogen peroxide feed distributor at the reaction heat removal component, and then flows through the heat exchange component 135 of the reaction heat removal component while flowing upward and undergoing an epoxidation reaction. The strong reaction heat released is quickly carried away by the cold source outlet pipe 134 of the reaction heat removal component, so that the reaction liquid is in a constant temperature reaction state, realizing rapid heat transfer. The reaction heat removal device 130 is an independent closed-loop cooling circuit system. After the reaction is complete, the reaction products and catalyst enter the separation device 150 at the top of the circulating fluidized reactor 120 for separation. The liquid-phase reaction products are collected from the top of the separation device 150 for product purification. The catalyst settles to the bottom of the separation device 150 by gravity and then flows into the buffer component 161 for stable enrichment. The bottom of the buffer component 161 is controlled by a valve, and a small portion of the catalyst is separated and enters the regeneration component 162 for catalyst regeneration. The catalyst is washed with methanol to restore its activity. The remaining catalyst and the regenerated catalyst enter the closed hopper at the same time. The closed hopper is used to control the circulation rate of the catalyst. The catalyst flowing out of the closed hopper is then lifted to the feed dispersion device 110 by the pressurization component 164 to complete the catalyst circulation.

[0051] This application features a constant reaction temperature, high hydrogen peroxide conversion rate, high PO selectivity, continuous regeneration, stable production, and long operating cycle, greatly improving the economic efficiency of the equipment operation. Specifically, this application has the following advantages:

[0052] 1. It achieves continuous and stable operation of propylene epoxidation reaction and deactivated catalyst regeneration, effectively maintains the stability of the reaction state, improves the selectivity of the target product, and greatly improves the system operation cycle and economy.

[0053] 2. The system adopts an upflow form from bottom to top. At the material inlet 120a, the reactant is close to a plug flow, which realizes enhanced mass and heat transfer, constant and uniform reaction temperature, high reaction conversion rate and product selectivity, and long catalyst life.

[0054] 3. The reaction heat removal component can quickly transfer the heat of reaction, maintain a stable reaction temperature, and prevent overheating.

[0055] 4. The feed dispersion device 110 disperses propylene into microdroplets, which has a large micro-interface mass transfer area, accelerating mass and heat transfer. The short contact time between the reactants and the catalyst effectively suppresses the occurrence of side reactions.

[0056] A second aspect of this application provides a method for using a circulating fluidized bed reactor system. Taking the production of propylene oxide as an example, the material entering through the end feed inlet 111b is methanol, the material entering through the side feed inlet 111c is propylene, and the material entering through the material inlet 120a is hydrogen peroxide. The catalyst is a TS-1 type titanium-silicon molecular sieve HPPO catalyst. The method of use includes:

[0057] S1. Start the reaction cooling device 130. Feed materials are introduced into the circulating fluidized reactor 120 through the feed dispersion device 110 and the material inlet 120a. The materials include the aforementioned methanol, propylene, hydrogen peroxide, and catalyst. Methanol is used as the washing medium, with a washing temperature of 20–50°C, preferably 25–35°C. The hydrogen peroxide concentration is 27.5 wt%–70 wt%, preferably 50%–60 wt%. The propylene / hydrogen peroxide molar ratio is 1.2–3:1, and the methanol / hydrogen peroxide molar ratio is 2.0–10:1. The catalyst also enters the feed dispersion device 110 simultaneously. The catalyst particles are small spheres with a diameter of 0.2–1.5 mm, preferably 0.5–1 mm. Propylene and methanol enter the circulating fluidized reactor 120 through the feed dispersion device 110, where they are pre-mixed with the catalyst. Hydrogen peroxide enters the circulating fluidized reactor 120 in stages from the side, where it undergoes an epoxidation reaction with the propylene under the action of the catalyst.

[0058] S2. The temperature in the reaction chamber 123 is adjusted by the reaction heat removal device 130. The heat generated by the reaction is transferred away by the reaction heat removal device 130, so that the temperature in the reaction chamber 123 is maintained at [20℃, 60℃], such as 20℃ and 60℃, preferably 25~35℃. The cold source is demineralized water. In an optional embodiment, when the circulating fluidized reaction cylinder 120 has multiple sections, the temperature of the cold source in the reaction heat removal device 130 corresponding to the lower section of the reaction cylinder 124 is lower than the temperature of the cold source in the reaction heat removal device 130 corresponding to the upper section of the reaction cylinder 125. For example, if a four-section circulating fluidized reaction cylinder 120 is used, from bottom to top, it is section one, section two, section three, and section four, corresponding to section one, section two, section three, and section four cold sources, respectively. Each section of cold source is circulated through a set of reaction heat removal devices 130 and can be controlled independently. The temperature of the first and second stage cold source medium is 0-20℃, preferably 5-15℃; the temperature of the third and fourth stage cold source medium is 25-45℃, preferably 30-40℃; and the pressure of the cold source medium is 0.4-1.0MPa, preferably 0.5-0.7MPa.

[0059] S3. Material is injected into the reaction chamber 123 through the feeding and dispersing device 110 and through the material inlet 120a, so that the pressure in the reaction chamber 123 is in the range of [1.6 MPa, 3.5 MPa], such as 1.6 MPa, 3.5 MPa, preferably 2.4 to 3.0 MPa, and the apparent flow rate of the material in the reaction chamber 123 is [0.02 m / s, 0.5 m / s], such as 0.02 m / s, 0.5 m / s, 0.05 to 0.3 m / s. The order of steps S3 and S2 can be interchanged.

[0060] S4. The reaction products and residues are separated by the separation device 150. After the reaction is completed, the reaction products and residues enter the separation device 150. The liquid phase is transferred out from the top of the separation device 150. The solid particulate catalyst enters the buffer component 161 under the action of gravity. The residues are then regenerated by the material circulation device 160. The regenerated catalyst is returned to the feed dispersion device 110 and mixed with the material again to complete the catalyst circulation. The aforementioned residue is the catalyst after the reaction. The catalyst may have partially lost its activity. The catalyst is regenerated through a material circulation device 160. Regenerated liquid is injected into the regeneration assembly 162 by connecting the high-temperature regeneration liquid inlet 162a and the low-temperature regeneration liquid inlet 162b, and discharged through the regeneration liquid outlet 162c. The regeneration liquid is methanol, but other liquids can also be used, adjusted according to the catalyst. In an optional embodiment, the temperature of the regeneration liquid introduced into the high-temperature regeneration liquid inlet 162a in the material circulation device 160 is [100℃, 150℃], and the temperature of the regeneration liquid introduced into the low-temperature regeneration liquid inlet 162b is [20℃, 60℃]. The pressure inside the regeneration assembly 162 is [2.0 MPa, 3.5 MPa]. Furthermore, when production stops or the catalyst reaches the end of its service life, the catalyst can be discharged through the discharge pipe 161a. When the amount of catalyst is insufficient, new catalyst can be added to the pressure barrier assembly 163 through the feeding section 163a to replenish the catalyst.

[0061] The use of existing chemical production equipment cannot solve the problem of timely elimination of local hot spots, resulting in poor production effect and efficiency, increased consumption of reactants and catalysts, high operating costs, and inability to achieve stable production. For example, in the production of propylene oxide, the tubular fixed-bed reactor used has poor heat and mass transfer between reactants and products, making it easy for local hot spots to form in the reaction area, leading to more side reactions and thus affecting production effect and efficiency. In contrast, this application uses a feeding dispersion device 110 and feed inlet 120a to add materials, maintaining the pressure in the reaction chamber 123 within a certain range and keeping the material at a certain flow rate. This facilitates material dispersion and contact, allowing the materials to react fully in the reaction chamber 123 without generating local hot spots. At the same time, by maintaining the temperature of the reaction chamber 123 within a certain range, side reactions are less likely to occur, and heat can be removed in time, which helps the formation of reaction products and reduces other byproducts, thereby improving production effect and efficiency. It also effectively utilizes reactants and catalysts, enabling the production equipment to operate efficiently and stably.

[0062] The technology of the present invention will be further explained below with reference to examples:

[0063] Example 1

[0064] use Figure 1 The circulating fluidized bed reactor system 100 includes a four-section circulating fluidized bed reactor 120, each section equipped with a heat exchange unit 135, such as heat exchange tubes. These heat exchange tubes are smooth and have a diameter of 25 mm. The cooling medium is circulating water. The reactants contain 99.6% propylene by volume, 50% hydrogen peroxide, and methanol as the solvent. The molar ratio of hydrogen peroxide to propylene to methanol is 1:2.5:5. The reactor temperature is 35℃, the reaction pressure is 2.5 MPa, and the apparent flow velocity of the liquid phase in the reactor is 0.1 m / s.

[0065] Example 2

[0066] The circulating fluidized bed reactor system 100 described above is used, wherein the circulating fluidized bed reactor 120 is configured in three sections, each section is equipped with one set of heat exchange components 135, such as heat exchange tubes. The heat exchange tubes are twisted tubes with a diameter of 25 mm, and the cooling medium is circulating water. The reactants have a propylene volume content of 99.6%, a hydrogen peroxide concentration of 50%, and methanol as the solvent. The molar ratio of hydrogen peroxide:propylene:methanol is 1:2.5:5. The reactor reaction temperature is 35℃, the reaction pressure is 2.5 MPa, and the apparent flow velocity of the liquid phase material in the reactor is 0.1 m / s.

[0067] Using the method described in this application, the conversion rate of hydrogen peroxide reaches 99.9%, the effective utilization rate reaches 99.99%, the selectivity of propylene oxide reaches over 99.5%, the reaction temperature rise can be controlled to no more than 1℃, continuous regeneration production operation is possible, long-cycle operation is possible, and good economic benefits are achieved. Compared with the existing fixed-bed tubular reactor process used in industrial applications, the reaction effect is significantly improved, and the specific results are shown in Table 1:

[0068] Table 1

[0069] Reaction pressure, MPa 2.5 2.5 2.7～3.3 Reaction temperature, °C 35 35 40～44 Hydrogen peroxide conversion rate, % 99.92 99.95 96.5 Hydrogen peroxide effective utilization rate, % 99.99 99.99 86.1 propylene oxide selectivity, % 99.55 99.67 97.8 Reaction temperature rise, ℃ 0.8 0.5 4

[0070] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," "optional example," or "optional implementation," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. In addition, those skilled in the art can combine and integrate the different embodiments or examples described in this specification.

[0071] Furthermore, the technical solutions of the various embodiments can be combined with each other, but only if they are based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed in this application.

[0072] Although embodiments of this application have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of this application, the scope of which is defined by the claims and their equivalents.

Claims

1. A circulating fluidized bed reactor system, characterized in that, include: A circulating fluidized bed reactor (120) has a lower end (121) for feeding and an upper end (122) for discharging, the upper end (122) being higher than the lower end (121). A material inlet (120a) is provided on the side of the circulating fluidized bed reactor (120). A reaction chamber (123) is provided inside the circulating fluidized bed reactor (120), connecting the upper end (122), the lower end (121), and the material inlet (120a). The reaction chamber (123) provides space for the reaction. Material entering the reaction chamber (123) through the material inlet (120a) reacts with material entering the reaction chamber (123) through the lower end (121), and is then discharged through the upper end (122). After entering the reaction chamber (123), the material flows in a fluid form, and the flow direction is consistent with the flow direction from the lower end (121) to the upper end (122). A feeding dispersion device (110) is connected to the lower end (121). The feeding dispersion device (110) is used to disperse the material and inject the dispersed material into the reaction chamber (123) through the lower end (121). The reaction heat removal device (130) is partially located in the reaction chamber (123) for heat exchange with the fluid in the reaction chamber (123); the other part is located outside the circulating fluidized reaction cylinder (120) for providing a cold source. A separation device (150) is used to separate the product. The separation device (150) is connected to the upper end (122). The separation device (150) is provided with a first outlet (151) for separating the product and a second outlet (152) for separating the residue. A material circulation device (160) is used to regenerate the separated residue and circulate it back to the feed dispersion device (110). One end of the material circulation device (160) is connected to the second outlet (152), and the other end is connected to the feed dispersion device (110). The feeding and dispersing device (110) includes a variable diameter section (111) and a mixing section (112). The mixing section (112) is connected to the lower end (121) and communicates with the material circulation device (160). One end of the variable diameter section (111) is provided with an end feed port (111b), and the opposite end of the variable diameter section (111) is communicated with the mixing section (112). The variable diameter section (111) has a through-hole... A fluid channel (111a) is provided at both ends. The diameter of the middle part of the fluid channel (111a) is smaller than the diameter of the two ends. The diameter of the fluid channel (111a) gradually changes from one end to the other end. The diameter-changing part (111) is also provided with a side feed port (111c). The side feed port (111c) is connected to the diameter-changing position of the fluid channel (111a) near the mixing part (112). There are multiple side feed ports (111c). The mixing section (112) includes a mixing component (113) and a baffle (114). The mixing component (113) is connected to the variable diameter section (111). The mixing component (113) has a plurality of holes for dispersing materials. The baffle (114) is located on the top of the mixing component (113). The baffle (114) blocks the holes located on the top of the mixing component (113) to prevent the holes from being blocked.

2. The circulating fluidized bed reactor system according to claim 1, characterized in that, The circulating fluidized bed reactor (120) is divided into multiple sections from the lower end (121) to the upper end (122). Each section of the circulating fluidized bed reactor (120) is provided with a material inlet (120a). The section closer to the lower end (121) is called the lower section reactor (124), and the section closer to the upper end (122) is called the upper section reactor (125). The length of the lower section reactor (124) is shorter than that of the upper section reactor (125).

3. The circulating fluidized bed reactor system according to claim 2, characterized in that, It also includes a segmented feeding device (140), which includes multiple segmented feeding pipes (141) and multiple feeding distribution components (142). The segmented feeding pipes (141) are respectively connected to each of the material ports (120a). The segmented feeding pipes (141) are connected to the feeding distribution components (142). The feeding distribution components (142) are located in the reaction chamber (123). Through the multiple segmented feeding pipes (141), the material can be injected into multiple sections of the circulating fluidized reaction cylinder (120).

4. The circulating fluidized bed reactor system according to claim 1, characterized in that, The reaction heat removal device (130) includes a cold source pressurization assembly (131), a cooling assembly (132), a cold source inlet pipe (133), a cold source outlet pipe (134), and a heat exchanger (135). The heat exchanger (135) is located inside the reaction chamber (123). The cold source inlet pipe (133) is connected to the inlet of the heat exchanger (135), and the cold source outlet pipe (134) is connected to the outlet of the heat exchanger (135), so that the heat exchanger... The cold source in the replacement component (135) flows in the opposite direction to the direction from the upper end (122) to the lower end (121). The cold source inlet pipe (133) is connected to the cooling component (132), and the cold source outlet pipe (134) is connected to the cold source pressurization component (131). The cold source pressurization component (131) is connected to the cooling component (132). The cold source pressurization component (131) is used to pressurize the cold source, and the cooling component (132) is used to cool the cold source.

5. The circulating fluidized bed reactor system according to claim 2, characterized in that, The material circulation device (160) includes components with progressively decreasing heights: A buffer assembly (161) is used to buffer the material. The buffer assembly (161) is lower than the separation device (150). The buffer assembly (161) is connected to the second outlet (152). The bottom of the buffer assembly (161) is provided with a discharge pipe (161a) for discharging the separation residue. The regeneration component (162) is used to regenerate the separated residue. The sidewall of the regeneration component (162) is provided with a high-temperature regeneration liquid inlet (162a), a regeneration liquid outlet (162c), and a low-temperature regeneration liquid inlet (162b) with decreasing heights. The top of the regeneration component (162) is connected to the buffer component (161). A pressure barrier assembly (163) is used to allow the separated residue to pass through and to block it in order to maintain the pressure difference. The top end of the pressure barrier assembly (163) is connected to the buffer assembly (161) and the regeneration assembly (162) respectively. The top end of the pressure barrier assembly (163) is also provided with a feeding part (163a) for replenishing materials. The bottom end of the pressure barrier assembly (163) is connected to the mixing part (112).

6. A method of using a circulating fluidized bed reactor system, characterized in that, The method of using the circulating fluidized reactor system according to any one of claims 1-5 includes: Start the reaction cooling device (130) and introduce materials into the circulating fluidized reaction cylinder (120) through the feed dispersion device (110) and the material port (120a); The temperature in the reaction chamber (123) is adjusted by the reaction cooling device (130) to maintain the temperature in the reaction chamber (123) at [20℃, 60℃]. Material is injected into the reaction chamber (123) through the feeding and dispersing device (110) and through the material port (120a), so that the pressure range in the reaction chamber (123) is [1.6 MPa, 3.5 MPa] and the apparent flow rate of the material in the reaction chamber (123) is [0.02 m / s, 0.5 m / s]. The reaction products and residues are separated by the separation device (150), and the residues are regenerated and returned to the feed dispersion device (110) by the material circulation device (160).

7. The method of using the circulating fluidized bed reactor system according to claim 6, characterized in that, When the circulating fluidized reaction cylinder (120) is provided with multiple sections, the temperature of the cold source in the reaction heat removal device (130) corresponding to the lower section reaction cylinder (124) is lower than the temperature of the cold source in the reaction heat removal device (130) corresponding to the upper section reaction cylinder (125).

8. The method of using the circulating fluidized bed reactor system according to claim 7, characterized in that, In the material circulation device (160), the temperature of the regenerated liquid introduced into the high-temperature regenerated liquid inlet (162a) is [100℃, 150℃], the temperature of the regenerated liquid introduced into the low-temperature regenerated liquid inlet (162b) is [20℃, 60℃], and the pressure inside the regeneration component (162) is [2.0Mpa, 3.5Mpa].

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