A continuous ethoxylation reaction apparatus

Abstract

The application relates to the technical field of ethoxylation product production equipment, in particular to a continuous ethoxylation reaction device. The continuous ethoxylation reaction device comprises a starting agent storage tank group, a catalyst storage tank, a mixing kettle, a combined monomer reactor group, an ethylene oxide storage tank, a propylene oxide storage tank and a post-treatment tank; the starting agent storage tank group is connected with the mixing kettle; the catalyst storage tank is connected with the mixing kettle; starting agent in the starting agent storage tank and catalyst in the catalyst storage tank are mixed in the mixing kettle and then transported to the combined monomer reactor group to perform ethoxylation reaction; the feeding end of the combined monomer reactor group is connected with the discharging end of the mixing kettle; and the feeding end of the ethylene oxide storage tank is connected with the feeding end of the combined monomer reactor group. The application can realize the continuity of the ethoxylation product production process, greatly improve the production efficiency compared with the batch kettle production, thereby reducing the production cost of the ethoxylation product and improving the core competitiveness of enterprises.

Description

Technical Field

[0001] This application relates to the field of equipment for the production of ethoxylated products, and in particular to a continuous ethoxylation reaction apparatus. Background Technology

[0002] The ethoxylation main unit is a production facility that carries out the ethoxylation reaction of initiators—hydrophobic raw materials (such as fatty alcohols, fatty acids, fatty amines, etc.)—with ethylene oxide (EO) and / or propylene oxide (PO). The working principle of the ethoxylation main unit is to produce ethoxylated products by reacting the initiators—hydrophobic raw materials—with ethylene oxide (EO) and / or propylene oxide (PO) in the presence of a catalyst. The catalyst can be an acidic catalyst, a basic catalyst, or a metal catalyst.

[0003] Current ethoxylation units in the prior art are typically batch production units consisting of a reaction vessel, feeding device, cooling device, separation device, and catalyst recovery device. However, current ethoxylation units cannot meet the requirements for continuous production of ethoxylated products, thus limiting the production efficiency and market price of ethoxylated products. Therefore, the applicant provides a continuous ethoxylation reaction apparatus. Summary of the Invention

[0004] To address the aforementioned technical problems, this application provides a continuous ethoxylation reaction apparatus.

[0005] The continuous ethoxylation reaction apparatus provided in this application is achieved through the following technical solution: A continuous ethoxylation reaction apparatus includes an initiator storage tank group, a catalyst storage tank, a mixing vessel, a combined monomer reactor group, an ethylene oxide storage tank, a propylene oxide storage tank, and a post-treatment tank. The initiator storage tank group comprises several initiator storage tanks, all of which are connected to the mixing vessel. The catalyst storage tank is connected to the mixing vessel. Accurately metered initiator from the initiator storage tanks and correctly metered catalyst from the catalyst storage tanks are mixed uniformly in the mixing vessel and then transported to the combined monomer reactor group for ethoxylation. The feed end of the combined monomer reactor group is connected to the discharge end of the mixing vessel. The feed end of the ethylene oxide storage tank is connected to the feed end of the combined monomer reactor group. The combined monomer reactor group comprises several monomer reactor unit components connected in series. The propylene oxide storage tank and the ethylene oxide storage tank are both connected to connecting pipelines between adjacent monomer reactor unit components. The feed end of the post-treatment tank is connected to the discharge end of the combined monomer reactor group and is used for neutralization and filtration to obtain the finished ethoxylated product.

[0006] This application enables the continuous production process of ethoxylated products, which greatly improves production efficiency compared to intermittent batch production, thereby reducing the production cost of ethoxylated products and enhancing the core competitiveness of enterprises.

[0007] Preferably, the bottom of the initiator storage tank is connected to a delivery branch pipe, and a first control valve and a first metering pump are sequentially arranged on the delivery branch pipe along the initiator delivery direction; a main delivery pipe is connected to the upper part of the periphery of the mixing vessel; the delivery branch pipe is fixedly connected to the periphery of the main delivery pipe; a second metering pump and a second control valve are sequentially arranged on the main delivery pipe along the initiator delivery direction, and the second metering pump is located downstream of the first metering pump; a packing pipe is connected to the bottom of the catalyst storage tank; a third control valve, a solid powder pipeline flow meter, and a fourth control valve are sequentially arranged on the packing pipe along the catalyst delivery direction; one end of the packing pipe is connected to the bottom of the catalyst storage tank and the other end is connected to the upper part of the periphery of the mixing vessel.

[0008] By adopting the above technical solution, the accurately metered starting agent and the correctly metered catalyst are mixed evenly in a mixing vessel and then transported to the combined monomer reactor group for ethoxylation reaction, which can ensure the quality of ethoxylated products while improving production efficiency.

[0009] Preferably, the bottom of the ethylene oxide storage tank is connected to an ethylene oxide transfer pipe; the ethylene oxide transfer pipe is sequentially equipped with a fifth control valve, a third metering pump, and a first temperature detector along the ethylene oxide transfer direction; the discharge end of the mixing vessel is connected to a mixture transfer pipe; the mixture transfer pipe is sequentially equipped with a sixth control valve, a fourth metering pump, and a second temperature detector along the mixture transfer direction; the feed end of the combined monomer reactor group is connected to a first mixer; the first mixer has two feed ports; one feed port of the first mixer is connected to the ethylene oxide transfer pipe; the other feed port of the first mixer is connected to the mixture transfer pipe of the mixing vessel.

[0010] By adopting the above technical solution, the temperature of the mixture in the input combined monomer reactor group can be precisely controlled, so as to achieve the optimal reaction conditions through commissioning, ensure the quality of ethoxylated products, and reduce process production costs.

[0011] Preferably, the first mixer includes a first manifold, a first delivery pump, and a first temperature control pipe. The first manifold has a Y-shaped flow channel inside. The Y-shaped flow channel includes a first mixture inlet channel, a first ethylene oxide inlet channel, and a first collecting channel. The first collecting channel is connected to the first mixture inlet channel and the first ethylene oxide inlet channel. The first collecting channel is filled with a first porous ceramic column. Helical rifling is formed inside the channels of the first porous ceramic column. The first manifold contains… A first mixing impeller is rotatably connected; the first mixing impeller is located at the common point of the first collecting channel, the first mixed material inlet channel, and the first ethylene oxide inlet channel; the liquid inlet end of the first delivery pump is connected to the discharge end of the first collecting channel in the first manifold; the liquid outlet end of the first delivery pump is connected to the inlet end of the first temperature control pipe; the first temperature control pipe is used to adjust and control the temperature of the liquid formed by the mixing of ethylene oxide delivered by the ethylene oxide storage tank and the mixed material delivered by the mixing vessel after passing through the first manifold and the first delivery pump.

[0012] By adopting the above technical solutions, the precise control performance of the temperature of the mixture in the input combined monomer reactor group can be further improved, the optimal reaction conditions can be obtained through commissioning, the quality of ethoxylated products can be guaranteed, and the process production cost can be reduced.

[0013] Preferably, the first temperature control pipe includes a copper alloy main pipe, a self-regulating heating wire, an aerogel felt, a porous buffer cotton, and a plastic outer tube. The self-regulating heating wire is spirally wound around the outer wall of the copper alloy main pipe; the aerogel felt covers the outer wall of the self-regulating heating wire; the porous buffer cotton covers the outer wall of the aerogel felt; the self-regulating heating wire, aerogel felt, and porous buffer cotton are all filled between the copper alloy main pipe and the plastic outer tube; a third temperature detector for detecting the material temperature is provided at both ends of the copper alloy main pipe; two jacket layers are formed inside the copper alloy main pipe, distributed at both ends of the copper alloy main pipe; each jacket layer is connected to a single heat exchange medium inlet pipe B and a single heat exchange medium outlet pipe B; a first centrifugal pump and a fourth temperature detector are provided on the heat exchange medium inlet pipe B. By controlling the flow rate of the first centrifugal pump, the temperature of the liquid in the copper alloy main pipe is adjusted, thereby ensuring the stability of the liquid temperature at the feed end of the combined unit reactor group, which is 65-75℃.

[0014] By adopting the above technical solutions, the precise control performance of the temperature of the mixture in the input combined monomer reactor group can be further improved, the optimal reaction conditions can be obtained through commissioning, the quality of ethoxylated products can be guaranteed, and the process production cost can be reduced.

[0015] Preferably, the single reactor unit assembly includes a reaction main tube and a heat exchange sleeve, the reaction main tube being fixedly connected inside the heat exchange sleeve; a heat exchange cavity is formed between the heat exchange sleeve and the reaction main tube; a heat exchange medium inlet pipe A is connected to the lower part of the heat exchange sleeve; a heat exchange medium outlet pipe A is connected to the upper part of the heat exchange sleeve; a guide pipe is fixedly connected inside the reaction main tube; one end of the guide pipe passes through the reaction main tube and is located outside the reaction main tube; another end of the guide pipe passes through the reaction main tube and is located at the bottom inside the reaction main tube; one end of the guide pipe located at the bottom inside the reaction main tube is open, and a flow channel gap is reserved between it and the bottom inside the reaction main tube; one end of the guide pipe located outside the reaction main tube is connected to a first temperature control pipe; a discharge pipe is connected to the periphery of the reaction main tube; the discharge pipe is located outside the heat exchange sleeve; the heat exchange medium flowing out of the heat exchange medium outlet pipe A is used to preheat ethylene oxide flowing out of the ethylene oxide storage tank and propylene oxide flowing out of the propylene oxide storage tank.

[0016] By adopting the above technical solutions, the multiple monomer combinations in this application can operate under different reaction temperatures, pressures, and other conditions as needed, achieving optimized reaction conditions through debugging, ensuring the quality of ethoxylated products while reducing process production costs. Furthermore, this application can precisely control the addition amount of EO / PO, yielding narrowly distributed ethoxylated products, and can also achieve EO / PO block production or heterogeneous end-capping, thereby obtaining polyether products with special properties. In addition, depending on the different EO / PO addition amounts, if the exothermic reaction exceeds the preheating requirements of the raw materials or the heat is insufficient, this application can remove or supplement the excess through a heat exchange medium.

[0017] Preferably, the individual reactor unit components are connected by a product communication pipeline; one end of the product communication pipeline is connected to the discharge pipe of the upstream individual reactor unit component and the other end is connected to the inlet end of the guide pipe of the downstream individual reactor unit component; the product communication pipeline is equipped with a fifth temperature detector, a second mixer, and a sixth temperature detector; the fifth temperature detector is located near the discharge pipe of the upstream individual reactor unit component; the sixth temperature detector is located near the guide pipe of the downstream individual reactor unit component; the second mixer is connected to an ethylene oxide storage tank and a propylene oxide storage tank; the second mixer is used to mix ethylene oxide, propylene oxide, and the material generated by the reaction of the upstream individual reactor unit component evenly; the propylene oxide storage tank is connected to a propylene oxide transfer pipe; the propylene oxide transfer pipe is connected to the product communication pipeline; the propylene oxide transfer pipe is equipped with a seventh control valve, a fifth metering pump, and a seventh temperature detector along the propylene oxide transfer direction.

[0018] By adopting the above technical solutions, the precise control performance of the temperature of the mixture in the input combined monomer reactor group can be further improved, the optimal reaction conditions can be obtained through commissioning, the quality of ethoxylated products can be guaranteed, and the process production cost can be reduced.

[0019] Preferably, the second mixer includes a second manifold, a second delivery pump, and a second temperature control pipe. The second manifold has a dendritic flow channel inside. The dendritic flow channel includes a second mixture feed channel connected to a product communication pipeline, a second ethylene oxide feed channel connected to an ethylene oxide storage tank, a propylene oxide feed channel connected to a propylene oxide storage tank, and a second collection channel connected to the liquid inlet end of the guide pipe of the downstream unit reactor assembly. The second collection channel is connected to the second mixture feed channel, the second ethylene oxide feed channel, and the propylene oxide feed channel. The second collection channel is filled with a second porous ceramic column. Helical rifling is formed inside the channels of the second porous ceramic column. A second mixing impeller is rotatably connected inside the second manifold. The second mixing impeller is located at the common point of the second collecting channel, the second mixed material inlet channel, the second ethylene oxide inlet channel, and the propylene oxide inlet channel; the liquid inlet end of the second delivery pump is connected to the discharge end of the second collecting channel in the second manifold; the liquid outlet end of the second delivery pump is connected to the inlet end of the second temperature control pipe; the second temperature control pipe is used to adjust and control the temperature of the liquid formed by mixing the ethylene oxide delivered by the ethylene oxide storage tank, the propylene oxide delivered by the propylene oxide storage tank, and the intermediate reaction production material delivered by the discharge pipe of the upstream monomer reactor unit component after passing through the second manifold and the second delivery pump, and to form ethoxylated polyether products with different block structures by controlling the mass ratio of the ethylene oxide delivered by the ethylene oxide storage tank and the propylene oxide delivered by the propylene oxide storage tank.

[0020] By adopting the above technical solutions, the precise control performance of the temperature of the mixture in the input combined monomer reactor group can be further improved, the optimal reaction conditions can be obtained through commissioning, the quality of ethoxylated products can be guaranteed, and the process production cost can be reduced.

[0021] Preferably, the inner and outer walls of the guide tube are integrally formed with a plurality of first heat dissipation strips that are consistent with the axial direction of the guide tube.

[0022] Preferably, the inner and outer walls of the reaction tube are integrally formed with several second heat dissipation strips that are aligned with the axial direction of the reaction tube.

[0023] By adopting the above technical solutions, the temperature control accuracy of the unit components of the single reactor can be improved, thereby ensuring product quality.

[0024] In summary, this application has the following advantages: 1. This application enables the continuous production process of ethoxylated products, which greatly improves production efficiency compared to intermittent batch production, thereby reducing the production cost of ethoxylated products and enhancing the core competitiveness of enterprises.

[0025] 2. The method for preparing ethoxylated products using the continuous ethoxylation reaction apparatus provided in this application is relatively simple and has a relatively low operational difficulty. By setting an appropriate aspect ratio, the mass transfer and heat transfer performance of a single reactor can be controlled. Different EO addition number requirements can be achieved through multiple combinations, which facilitates industrial production and manufacturing while meeting the customized design and production of products.

[0026] 3. In this application, multiple combined monomers can be operated under different reaction temperatures, pressures, and other conditions as needed to achieve optimal reaction conditions through debugging, ensuring the quality of ethoxylated products while reducing process production costs.

[0027] 4. This application can precisely control the amount of EO / PO addition, resulting in a narrow distribution of ethoxylated products.

[0028] 5. This application can effectively utilize the exothermic reaction, thereby achieving its own heat utilization through heat exchange between cold raw materials and reactants, reducing energy consumption, ensuring the quality of ethoxylated products, and reducing process production costs.

[0029] 6. Depending on the amount of EO / PO addition, if the heat generated exceeds the preheating requirements of the raw materials or is insufficient, the excess heat can be removed or supplemented by a heat exchange medium.

[0030] 7. This application can realize EO / PO block production or heterogeneous end-capping, thereby obtaining polyether products with special properties. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the overall structure of Embodiment 1 of this application.

[0032] Figure 2 This is a schematic diagram of the connection structure of the initiator storage tank group, catalyst storage tank and mixing vessel in Embodiment 1 of this application.

[0033] Figure 3 This is a schematic diagram of the connection structure between the mixing vessel and the ethylene oxide storage tank in an embodiment of this application.

[0034] Figure 4 This is a schematic diagram of the structure of the first mixer in the embodiments of this application.

[0035] Figure 5 yes Figure 4 A magnified view of a portion of point A in the middle.

[0036] Figure 6This is a schematic diagram of the structure of a single reactor unit component in an embodiment of this application.

[0037] Figure 7 This is a cross-sectional view of a single reactor unit component in an embodiment of this application.

[0038] Figure 8 This is a schematic diagram of the connection structure between the propylene oxide storage tank and the second mixer in an embodiment of this application.

[0039] Figure 9 This is a schematic diagram of the pipeline connection structure between the individual reactor unit components in the embodiments of this application.

[0040] Figure 10 This is a schematic diagram of the structure of the second mixer in the embodiments of this application.

[0041] In the diagram, 1. Initiator storage tank group; 11. Delivery branch pipe; 111. First control valve; 112. First metering pump; 12. Delivery main pipe; 121. Second metering pump; 122. Second control valve; 2. Catalyst storage tank; 21. Packing pipe; 22. Third control valve; 23. Solid powder pipeline flow meter; 24. Fourth control valve; 3. Mixing vessel; 31. Mixture transfer pipe; 311. Sixth control valve; 312. Fourth metering pump; 313. Second temperature detector; 4. Combined single reactor group; 40. Single reactor unit component; 400. Heat exchanger. Chamber; 401, Reaction Main Tube; 4011, Second Heat Dissipation Bar; 402, Heat Exchanger Sheath; 4021, Heat Exchanger Medium Inlet Pipe A; 4022, Heat Exchanger Medium Outlet Pipe A; 403, Guide Pipe; 4031, First Heat Dissipation Bar; 404, Discharge Pipe; 5, Ethylene Oxide Storage Tank; 51, Ethylene Oxide Transfer Pipe; 511, Fifth Control Valve; 512, Third Metering Pump; 513, First Temperature Detector; 6, Propylene Oxide Storage Tank; 61, Propylene Oxide Transfer Pipe; 611, Seventh Control Valve; 612, Fifth Metering Pump; 613, Seventh Temperature Detector; 7, Post-processing Tank; 8 81. First mixer; 810. First manifold; 811. "Y"-shaped flow channel; 812. First feed channel for mixed materials; 813. First ethylene oxide feed channel; 814. First collection channel; 815. First porous ceramic column; 816. First mixing impeller; 82. First transfer pump; 83. First temperature control pipe; 831. Copper alloy main pipe; 8310. Third temperature detector; 8311. Jacket layer; 8312. Heat exchange medium inlet pipe B; 8313. Heat exchange medium outlet pipe B; 8314. First centrifugal pump; 8315. Fourth temperature detector; 832. Self-limiting... 833. Heat tracing wire; 834. Aerogel felt; 835. Porous buffer cotton; 836. Plastic outer tube; 9. Product connecting pipe; 91. Fifth temperature detector; 92. Second mixer; 921. Second manifold; 9210. Dendritic flow channel; 9211. Second mixture feed channel; 9212. Second ethylene oxide feed channel; 9213. Propylene oxide feed channel; 9214. Second collection channel; 9215. Second ceramic porous column; 9216. Second mixing impeller; 922. Second delivery pump; 923. Second temperature control fitting; 93. Sixth temperature detector. Detailed Implementation

[0042] To further understand the present invention, preferred embodiments are described below with reference to examples. However, it should be understood that these descriptions are merely for illustrating the features and advantages of the present invention and are not intended to limit the scope of the claims. Those skilled in the art can refer to the content of this document to appropriately modify process parameters and corresponding conventional equipment components for implementation. Example

[0043] refer to Figure 1 This application discloses a continuous ethoxylation reaction apparatus comprising an initiator storage tank group 1, a catalyst storage tank 2, a mixing vessel 3, a combined monomer reactor group 4, an ethylene oxide storage tank 5, a propylene oxide storage tank 6, and a post-processing tank 7. The initiator storage tank group 1 includes several initiator storage tanks 10 storing different initiators, all of which are connected to the mixing vessel 3. The catalyst storage tank 2 is connected to the mixing vessel 3. Based on the initiator content input to the mixing vessel 3, the catalyst storage tank 2 metered and added the corresponding catalyst to the mixing vessel 3 for homogenization to obtain an initial mixture. The feed end of the combined monomer reactor group 4 is connected to the discharge end of the mixing vessel 3. That is, the accurately metered initiator in the initiator storage tank 10 and the correctly metered catalyst in the catalyst storage tank 2 are mixed evenly in the mixing vessel 3 and then transported to the combined monomer reactor group 4 for the ethoxylation reaction. The feed end of the ethylene oxide storage tank 5 is connected to the feed end of the combined monomer reactor group 4, where ethylene oxide and the initial mixture undergo an ethoxylation reaction. The combined monomer reactor group 4 comprises several monomer reactor unit components 40 connected in series. Propylene oxide storage tank 6 and ethylene oxide storage tank 5 are both connected to the connecting pipelines between adjacent monomer reactor unit components 40. An intermediate material formed by ethylene oxide and the initial mixture is mixed evenly with a specific ratio of ethylene oxide / propylene oxide before being placed in the monomer reactor unit component 40 for reaction, ultimately yielding the ethoxylated crude product. The feed end of the post-treatment tank 7 is connected to the discharge end of the combined monomer reactor group 4. The ethoxylated crude product output from the combined monomer reactor group 4 undergoes neutralization and filtration in the post-treatment tank 7 to obtain the finished ethoxylated product.

[0044] refer to Figure 1 and Figure 2Taking a single initiator storage tank 10 as an example, the connection structure between the initiator storage tank 10 and the mixing vessel 3 is illustrated. A delivery branch pipe 11 is coaxially and fixedly connected to the bottom center of the initiator storage tank 10. A first control valve 111 and a first metering pump 112 are sequentially installed on the delivery branch pipe 11 along the initiator delivery direction. The first control valve 111 is preferably a solenoid valve. A main delivery pipe 12 is fixedly connected to the upper periphery of the mixing vessel 3. The delivery branch pipe 11 is uniformly and fixedly connected to the upper periphery of the main delivery pipe 12 via flanges, meaning the central axis of the outlet end of the delivery branch pipe 11 is perpendicular to the central axis of the main delivery pipe 12. A second metering pump 121 and a second control valve 122 are sequentially installed on the main delivery pipe 12 along the initiator delivery direction. The second control valve 122 is preferably a solenoid valve. The second metering pump 121 is located downstream of the first metering pump 112 and near the connection end between the mixing vessel 3 and the main conveying pipe 12. The second metering pump 121 is used to meter the volume of the initiator input into the mixing vessel 3, and the mass of the initiator input into the mixing vessel 3 is obtained using the formula M (mass) = V*ρ. Based on the mass of the initiator input into the mixing vessel 3, the mass of the catalyst input into the mixing vessel 3 is measured. The catalyst storage tank 2 has a packing pipe 21 coaxially and fixedly connected to its bottom center. Along the catalyst conveying direction, the packing pipe 21 is sequentially equipped with a third control valve 22, a solid powder pipeline flow meter 23, and a fourth control valve 24. The third control valve 22 and the fourth control valve 24 are preferably solenoid valves. One end of the packing pipe 21 is fixedly connected to the bottom center of the catalyst storage tank 2, and the other end is fixedly connected to the upper periphery of the mixing vessel 3. By metering with the solid powder pipeline flow meter 23, the mass of the catalyst input into the mixing vessel 3 can be controlled, improving the production quality stability of the entire ethoxylation reaction unit.

[0045] refer to Figure 1 and Figure 3 The bottom center of the ethylene oxide storage tank 5 is coaxially and fixedly connected to an ethylene oxide transfer pipe 51. Along the ethylene oxide transfer direction, a fifth control valve 511, a third metering pump 512, and a first temperature detector 513 are sequentially installed on the ethylene oxide transfer pipe 51. The fifth control valve 511 is preferably a solenoid valve. The discharge end of the mixing vessel 3 is fixedly connected to a mixture transfer pipe 31. Along the mixture transfer direction, a sixth control valve 311, a fourth metering pump 312, and a second temperature detector 313 are sequentially installed on the mixture transfer pipe 31. The sixth control valve 311 is preferably a solenoid valve. The feed end of the combined unit reactor group 4 is fixedly connected to a first mixer 8 for uniformly mixing the initial mixture and ethylene oxide. The first mixer 8 is machined to have two feed ports. One feed port of the first mixer 8 is fixedly connected to the ethylene oxide transfer pipe 51. The other feed port of the first mixer 8 is fixedly connected to the mixture transfer pipe 31 of the mixing vessel 3. The discharge port of the first mixer 8 is fixedly connected to the feed port of the combined single reactor group 4.

[0046] refer to Figure 1 and Figure 4 The first mixer 8 includes a first manifold 81 for uniformly mixing the initial mixture and ethylene oxide, a first delivery pump 82 for controlling the flow rate of the liquid material input to the combined monomer reactor group 4, and a first temperature control pipe 83 for controlling the temperature of the liquid material obtained by uniformly mixing the initial mixture and ethylene oxide.

[0047] refer to Figure 1 and Figure 4 The first manifold 81 has a Y-shaped flow channel 810 inside. The Y-shaped flow channel 810 can be divided into a first mixture feed channel 811, a first ethylene oxide feed channel 812, and a first collecting channel 813. The first collecting channel 813 is connected to the first mixture feed channel 811 and the first ethylene oxide feed channel 812. The angle formed by the central axis of the first mixture feed channel 811 and the central axis of the first ethylene oxide feed channel 812 is 40-120°, preferably 80-120°. The first collecting channel 813 is filled with a first porous ceramic column 814 for tempering. The internal channels of the first porous ceramic column 814 are integrally machined to form helical rifling. A first mixing impeller 815 is rotatably connected inside the first manifold 81, located at the common point of the first collecting channel 813, the first mixed material inlet channel 811, and the first ethylene oxide inlet channel 812, facilitating thorough and uniform mixing of the liquid materials. The inlet end of the first delivery pump 82 is connected to the outlet end of the first collecting channel 813 in the first manifold 81, and the outlet end of the first delivery pump 82 is connected to the inlet end of the first temperature control pipe 83, while the outlet end of the first temperature control pipe 83 is fixedly connected to the inlet end of the combined single reactor group 4.

[0048] refer to Figure 1 and Figure 4 The first temperature control pipe 83 is used to adjust and control the temperature of the liquid formed by the mixing of ethylene oxide conveyed by the ethylene oxide storage tank 5 and the mixture conveyed by the mixing vessel 3 after passing through the first manifold 81 and the first delivery pump 82. It can then be operated under different reaction temperatures, pressures and other conditions as needed to achieve the optimal reaction conditions through debugging, ensure the quality of ethoxylated products and reduce process production costs.

[0049] refer to Figure 4 and Figure 5The first temperature-controlled pipe fitting 83 includes a copper alloy main pipe 831, a self-regulating heat tracing wire 832, an aerogel felt 833, a porous buffer cotton 834, and a plastic outer tube 835. The self-regulating heat tracing wire 832, aerogel felt 833, and porous buffer cotton 834 are all filled between the copper alloy main pipe 831 and the plastic outer tube 835. The self-regulating heat tracing wire 832 is spirally wound around the outer wall of the copper alloy main pipe 831, serving to maintain a stable temperature of the liquid inside the first temperature-controlled pipe fitting 83. It mainly addresses situations where the liquid's heat is insufficient, supplementing the liquid with heat to ensure a stable temperature of the liquid entering the first temperature-controlled pipe fitting 83. The aerogel felt 833 covers the outer wall of the self-regulating heat tracing wire 832, and the porous buffer cotton 834 covers the outer wall of the aerogel felt 833. Both primarily serve to fill, insulate, and provide insulation, fully utilizing thermal energy and reducing production energy consumption.

[0050] refer to Figure 1 and Figure 4 To address excessive heat in the liquid, a third temperature sensor 8310 for detecting the material temperature is installed at both ends of the copper alloy main pipe 831. Two jacket layers 8311 are formed inside the copper alloy main pipe 831, distributed at both ends. Each jacket layer 8311 is fixedly connected to a single heat exchange medium inlet pipe B8312 and a single heat exchange medium outlet pipe B8313. The heat exchange medium inlet pipe B8312 is fixedly connected to the lower bottom of the copper alloy main pipe 831, and the heat exchange medium outlet pipe B8313 is fixedly connected to the upper top of the copper alloy main pipe 831. A first centrifugal pump 8314 and a fourth temperature sensor 8315 are installed on the heat exchange medium inlet pipe B8312. By controlling the flow rate of the first centrifugal pump 8314, the temperature of the liquid in the copper alloy main pipe 831 can be adjusted, thereby ensuring the temperature stability of the liquid entering the feed end of the combined single reactor group 4. In this application, the liquid temperature at the feed end of the combined single reactor group 4 is 65-75°C, and preferably 70°C.

[0051] refer to Figure 1 and Figure 6The single reactor unit component 40 includes a reaction main pipe 401, a heat exchange sleeve 402, and a guide pipe 403. The reaction main pipe 401 is fixedly connected inside the heat exchange sleeve 402, with one end extending beyond the heat exchange sleeve 402 and located outside it. The heat exchange sleeve 402 is mainly used to control the reaction temperature of the mixture. A heat exchange cavity 400 is formed between the heat exchange sleeve 402 and the reaction main pipe 401, and the heat exchange medium flows through the heat exchange cavity 400. A heat exchange medium inlet pipe A4021 is fixedly connected to the lower part of the heat exchange sleeve 402, while a heat exchange medium outlet pipe A4022 is fixedly connected to the upper part of the heat exchange sleeve 402. The reaction temperature of the mixture can be controlled by controlling the flow rate and temperature of the heat exchange medium. A guide pipe 403 is inserted into the main reaction tube 401, with one end of the guide pipe 403 passing through the main reaction tube 401 and located outside the main reaction tube 401; the other end of the guide pipe 403 passes through the main reaction tube 401 and is located at the bottom inside the main reaction tube 401. One end of the guide pipe 403 located at the bottom inside the main reaction tube 401 is open, and a flow channel gap is reserved between it and the bottom inside the main reaction tube 401. One end of the guide pipe 403 located outside the main reaction tube 401 is coaxially and fixedly connected to the first temperature control pipe 83. A discharge pipe 404 located outside the heat exchange sleeve 402 is fixedly connected to the bottom periphery of the main reaction tube 401, and the discharge pipe 404 is connected to the feed end of the downstream single reactor unit assembly 40. The reaction in the unit reactor 40 is exothermic. The heat exchange medium flowing out of the heat exchange medium outlet pipe A4022 can be used to preheat the ethylene oxide flowing out of the ethylene oxide storage tank 5 and the propylene oxide flowing out of the propylene oxide storage tank 6. By making full use of the heat of reaction, the overall production energy consumption of this application can be reduced, thereby reducing the production cost of the ethoxylated product, which is in line with the concept of environmental protection and development.

[0052] refer to Figure 1 and Figure 7 To improve the controllability of the heat exchanger sleeve 402, several first heat dissipation strips 4031, aligned axially with the inner and outer walls of the guide tube 403, are integrally formed. These first heat dissipation strips 4031 are uniformly arranged around the central axis of the guide tube 403 and fixedly connected to its inner and outer walls. (Reference) Figure 1 To further enhance the control performance of the heat exchanger sleeve 402, several second heat dissipation strips 4011, which are aligned with the axial direction of the reaction main tube 401, are integrally formed on both the inner and outer walls of the reaction main tube 401. The second heat dissipation strips 4011 are also uniformly wrapped around the central axis of the reaction main tube 401 and fixedly connected to the inner and outer walls of the reaction main tube 401.

[0053] refer to Figure 1 and Figure 8The bottom of the propylene oxide storage tank 6 is coaxially and fixedly connected to a propylene oxide transfer pipe 61. Along the propylene oxide transfer direction, a seventh control valve 611, a fifth metering pump 612, and a seventh temperature detector 613 are installed on the propylene oxide transfer pipe 61. The seventh control valve 611 is preferably a solenoid valve.

[0054] refer to Figure 1 and Figure 9 A product connecting pipe 9 connects adjacent individual reactor unit components 40, and a propylene oxide transfer pipe 61 is connected to the product connecting pipe 9. One end of the product connecting pipe 9 is fixedly connected to the discharge pipe 404 of the upstream individual reactor unit component 40, and the other end is fixedly connected to the inlet end of the guide pipe 403 of the downstream individual reactor unit component 40. Along the material flow direction, the product connecting pipe 9 is equipped with a fifth temperature detector 91, a second mixer 92 for mixing ethylene oxide, propylene oxide, and the material generated by the reaction of the upstream individual reactor unit component 40, and a sixth temperature detector 93. The propylene oxide transfer pipe 61 is specifically connected to the second mixer 92. The fifth temperature detector 91 is located near the discharge pipe 404 of the upstream individual reactor unit component 40 and is used to detect the stability of the intermediate reactants output by the upstream individual reactor unit component 40, thereby facilitating temperature adjustment by the second mixer 92. The sixth temperature detector 93 is located near the guide pipe 403 of the downstream single-unit reactor component 40, allowing for a direct view of the material temperature input to the next single-unit reactor component 40 after temperature adjustment by the second mixer 92. The second mixer 92 is connected to both the ethylene oxide storage tank 5 and the propylene oxide storage tank 6, enabling the adjustment of the ethylene oxide / propylene oxide addition ratio to obtain ethoxylated polyether products with different block structures.

[0055] refer to Figure 1 and Figure 10 The specific structure of the second mixer 92 is as follows: The second mixer 92 includes a second manifold 921, a second delivery pump 922, and a second temperature control pipe 923 with the same structure as the first temperature control pipe 83. The second manifold 921 has a dendritic flow channel 9210 formed inside. Specifically, the dendritic flow channel 9210 includes a second mixture feed channel 9211 connected to the product communication pipe 9, a second ethylene oxide feed channel 9212 connected to the ethylene oxide storage tank 5, a propylene oxide feed channel 9213 connected to the propylene oxide storage tank 6, and a second collecting channel 9214 connected to the liquid inlet end of the guide pipe 403 of the downstream single reactor unit component 40. That is, the second collecting channel 9214 is connected to the second mixture feed channel 9211, the second ethylene oxide feed channel 9212, and the propylene oxide feed channel 9213.

[0056] refer to Figure 1 and Figure 10 The second collecting channel 9214 is filled with a second porous ceramic column 9215, and the internal channels of the second porous ceramic column 9215 form helical rifling. A second mixing impeller 9216 is rotatably connected within the second manifold 921, located at the common point between the second collecting channel 9214 and the second mixture feed channel 9211, the second ethylene oxide feed channel 9212, and the propylene oxide feed channel 9213. This facilitates uniform mixing of the materials input into the second mixer 92, ensuring the quality of the prepared ethoxylated product and its production efficiency. The inlet end of the second delivery pump 922 is connected to the outlet end of the second collecting channel 9214 in the second manifold 921. The outlet end of the second delivery pump 922 is also connected to the inlet end of the second temperature control pipe 923, which is fixedly connected to the guide pipe 403 of the single reactor unit assembly 40. The second transfer pump 922 is used to control the flow rate of the mixture, thereby adjusting the time it takes for the mixture to pass through the monomer reactor unit component 40. This allows for operation under different reaction temperatures and pressures as needed, achieving optimized reaction conditions through debugging, ensuring the quality of the ethoxylated product while reducing process production costs. The second temperature control pipe 923 is used to adjust and control the temperature of the liquid formed by the mixing of ethylene oxide from the ethylene oxide storage tank 5, propylene oxide from the propylene oxide storage tank 6, and intermediate reaction material from the discharge pipe 404 of the upstream monomer reactor unit component 40, after passing through the second manifold 921 and the second transfer pump 922. By controlling the mass ratio of ethylene oxide from the ethylene oxide storage tank 5 to the propylene oxide from the propylene oxide storage tank 6, ethoxylated polyether products with different block structures can be formed.

[0057] In summary, this application enables continuous production of ethoxylated products, significantly improving production efficiency compared to batch reactor production, thereby reducing production costs and enhancing the core competitiveness of enterprises. The method for preparing ethoxylated products using the continuous ethoxylation reactor provided in this application is relatively simple and easy to implement. By setting an appropriate aspect ratio, the mass and heat transfer performance of a single reactor can be controlled, and multiple combinations can achieve different EO addition number requirements, facilitating industrial-scale manufacturing while also meeting customized product design and production needs. Furthermore, the multiple monomer combinations in this application can be operated under different reaction temperatures, pressures, and other conditions as needed to achieve optimal reaction conditions through debugging, ensuring the quality of ethoxylated products while reducing process production costs. It can also precisely control the addition amount of EO / PO, resulting in narrowly distributed ethoxylated products. It can also effectively utilize the exothermic reaction by exchanging heat between cold raw materials and reactants to achieve its own heat utilization, reducing energy consumption and ensuring the quality of ethoxylated products while reducing process production costs. It can also achieve EO / PO block production or heterogeneous end-capping, thereby obtaining polyether products with special properties to meet customized needs.

[0058] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A continuous ethoxylation reaction apparatus, characterized in that: The reactor includes an initiator storage tank group (1), a catalyst storage tank (2), a mixing vessel (3), a combined monomer reactor group (4), an ethylene oxide storage tank (5), a propylene oxide storage tank (6), and a post-processing tank (7). The initiator storage tank group (1) includes several initiator storage tanks (10), all of which are connected to the mixing vessel (3). The catalyst storage tank (2) is connected to the mixing vessel (3). The accurately metered initiator in the initiator storage tank (10) and the correctly metered catalyst in the catalyst storage tank (2) are mixed evenly in the mixing vessel (3) and then transported to the combined monomer reactor group (4) for ethoxylation reaction. The feed end of the combined monomer reactor group (4) is connected to the outlet of the mixing vessel (3). The feed end is connected; the feed end of the ethylene oxide storage tank (5) is connected to the feed end of the combined monomer reactor group (4); the combined monomer reactor group (4) includes several monomer reactor unit components (40) connected in series, and the propylene oxide storage tank (6) and the ethylene oxide storage tank (5) are both connected to the connecting pipeline between adjacent monomer reactor unit components (40); the feed end of the post-treatment tank (7) is connected to the discharge end of the combined monomer reactor group (4) for neutralization and filtration to obtain the finished ethoxylated product; the bottom of each initiator storage tank (10) is connected to a conveying branch pipe (11), and the conveying branch pipe (11) is sequentially provided with a first control valve (111) and a first metering pump (111) along the initiator conveying direction. 112); The upper part of the periphery of the mixing vessel (3) is connected to the conveying main pipe (12); The conveying branch pipe (11) is fixedly connected to the periphery of the conveying main pipe (12); The conveying main pipe (12) is sequentially provided with a second metering pump (121) and a second control valve (122) along the initiator conveying direction, and the second metering pump (121) is located downstream of the first metering pump (112); The bottom of the catalyst storage tank (2) is connected to a packing pipe (21); The packing pipe (21) is sequentially provided with a third control valve (22), a solid powder pipeline flow meter (23), and a fourth control valve (24) along the catalyst conveying direction; One end of the packing pipe (21) is connected to the bottom of the catalyst storage tank (2) and the other end is connected to the The upper part of the periphery of the mixing vessel (3); the feed end of the combined single reactor group (4) is connected to a first mixer (8); the first mixer (8) includes a first manifold (81), a first delivery pump (82), and a first temperature control pipe (83), and a "y"-shaped flow channel (810) is formed inside the first manifold (81); the "y"-shaped flow channel (810) includes a first mixture feed channel (811), a first ethylene oxide feed channel (812), and a first collection channel (813), and the first collection channel (813) is connected to the first mixture feed channel (811) and the first ethylene oxide feed channel (812); the first collection channel (813) is filled with a first ceramic porous column (814).The first ceramic porous column (814) has spiral rifling inside its internal channels; a first mixing impeller (815) is rotatably connected inside the first manifold (81); the first mixing impeller (815) is located at the common point of the first collecting channel (813), the first mixed material feed channel (811), and the first ethylene oxide feed channel (812); the inlet end of the first delivery pump (82) is connected to the outlet end of the first collecting channel (813) in the first manifold (81); the outlet end of the first delivery pump (82) is connected to the inlet end of the first temperature control pipe (83); the first temperature control pipe (83) is used to adjust and control the temperature of the liquid formed by the mixing of ethylene oxide delivered by the ethylene oxide storage tank (5) and the mixed material delivered by the mixing vessel (3) after passing through the first manifold (81) and the first delivery pump (82).

2. The continuous ethoxylation reaction apparatus according to claim 1, characterized in that: The bottom of the ethylene oxide storage tank (5) is connected to an ethylene oxide transmission pipe (51); the ethylene oxide transmission pipe (51) is sequentially equipped with a fifth control valve (511), a third metering pump (512), and a first temperature detector (513) along the ethylene oxide transmission direction; the discharge end of the mixing vessel (3) is connected to a mixture transmission pipe (31); the mixture transmission pipe (31) is sequentially equipped with a sixth control valve (311), a fourth metering pump (312), and a second temperature detector (313) along the mixture transmission direction; the first mixer (8) has two feed ports; one feed port of the first mixer (8) is connected to the ethylene oxide transmission pipe (51); the other feed port of the first mixer (8) is connected to the mixture transmission pipe (31) of the mixing vessel (3).

3. The continuous ethoxylation reaction apparatus according to claim 1, characterized in that: The first temperature control fitting (83) includes a copper alloy main pipe (831), a self-regulating heating wire (832), an aerogel felt (833), a porous buffer cotton (834), and a plastic outer tube (835). The self-regulating heating wire (832) is spirally wound around the outer wall of the copper alloy main pipe (831). The aerogel felt (833) covers the outer wall of the self-regulating heating wire (832). The porous buffer cotton (834) covers the outer wall of the aerogel felt (833). The self-regulating heating wire (832), aerogel felt (833), and porous buffer cotton (834) are all filled between the copper alloy main pipe (831) and the plastic outer tube (835). The copper alloy main pipe (831) is provided with a third temperature sensor at both ends for detecting the temperature of the material. Instrument (8310); The copper alloy main pipe (831) has two jacket layers (8311) distributed at both ends of the copper alloy main pipe (831); Each jacket layer (8311) is connected to a single heat exchange medium inlet pipe B (8312) and a single heat exchange medium outlet pipe B (8313); The heat exchange medium inlet pipe B (8312) is equipped with a first centrifugal pump (8314) and a fourth temperature detector (8315). By controlling the flow rate of the first centrifugal pump (8314), the temperature of the liquid in the copper alloy main pipe (831) is adjusted, thereby ensuring the stability of the liquid temperature at the feed end of the input combined single reactor group (4). The liquid temperature at the feed end of the input combined single reactor group (4) is 65-75℃.

4. The continuous ethoxylation reaction apparatus according to claim 3, characterized in that: The single reactor unit assembly (40) includes a reaction main tube (401) and a heat exchange sleeve (402). The reaction main tube (401) is fixedly connected inside the heat exchange sleeve (402). A heat exchange cavity (400) is formed between the heat exchange sleeve (402) and the reaction main tube (401). A heat exchange medium inlet pipe A (4021) is connected to the lower part of the heat exchange sleeve (402). A heat exchange medium outlet pipe A (4022) is connected to the upper part of the heat exchange sleeve (402). A guide pipe (403) is fixedly connected inside the reaction main tube (401). One end of the guide pipe (403) passes through the reaction main tube (401) and is located outside the reaction main tube (401). The reaction main tube (401) is located at the bottom of the reaction main tube (401); one end of the guide tube (403) located at the bottom of the reaction main tube (401) is open and a flow channel gap is reserved between it and the bottom of the reaction main tube (401); one end of the guide tube (403) located outside the reaction main tube (401) is connected to the first temperature control pipe (83); the reaction main tube (401) is connected to the discharge pipe (404) on its periphery; the discharge pipe (404) is located outside the heat exchange sleeve (402); the heat exchange medium flowing out of the heat exchange medium outlet pipe A (4022) is used to preheat the ethylene oxide flowing out of the ethylene oxide storage tank (5) and the propylene oxide flowing out of the propylene oxide storage tank (6).

5. A continuous ethoxylation reaction apparatus according to claim 4, characterized in that: A product communication pipeline (9) connects adjacent individual reactor unit components (40); one end of the product communication pipeline (9) is connected to the discharge pipe (404) of the upstream individual reactor unit component (40) and the other end is connected to the inlet end of the guide pipe (403) of the downstream individual reactor unit component (40); the product communication pipeline (9) is equipped with a fifth temperature detector (91), a second mixer (92), and a sixth temperature detector (93); the fifth temperature detector (91) is located near the discharge pipe (404) of the upstream individual reactor unit component (40); the sixth temperature detector (93) is located near the downstream individual reactor unit component (40). The reactor unit assembly (40) has a flow guide pipe (403); the second mixer (92) is connected to the ethylene oxide storage tank (5) and the propylene oxide storage tank (6); the second mixer (92) is used to mix the ethylene oxide, propylene oxide and the material generated by the reaction of the upstream single reactor unit assembly (40) evenly; the propylene oxide storage tank (6) is connected to the propylene oxide transmission pipe (61); the propylene oxide transmission pipe (61) is connected to the product communication pipe (9); the propylene oxide transmission pipe (61) is equipped with a seventh control valve (611), a fifth metering pump (612) and a seventh temperature detector (613) along the propylene oxide transmission direction.

6. The continuous ethoxylation reaction apparatus according to claim 5, characterized in that: The second mixer (92) includes a second manifold (921), a second delivery pump (922), and a second temperature control pipe (923). The second manifold (921) has a dendritic flow channel (9210) inside. The dendritic flow channel (9210) includes a second mixture feed channel (9211) connected to the product communication pipeline (9), a second ethylene oxide feed channel (9212) connected to the ethylene oxide storage tank (5), an ethylene oxide feed channel (9213) connected to the propylene oxide storage tank (6), and a downstream... The inlet end of the guide pipe (403) of the single reactor unit component (40) is connected to the second collecting channel (9214), which is connected to the second mixture feed channel (9211), the second ethylene oxide feed channel (9212), and the propylene oxide feed channel (9213). The second collecting channel (9214) is filled with a second ceramic porous column (9215). The internal channels of the second ceramic porous column (9215) form a spiral rifling. The second manifold (921) rotates within the second manifold. A second mixing impeller (9216) is connected; the second mixing impeller (9216) is located at the common point of the second collecting channel (9214), the second mixture feed channel (9211), the second ethylene oxide feed channel (9212), and the propylene oxide feed channel (9213); the liquid inlet of the second delivery pump (922) is connected to the discharge end of the second collecting channel (9214) in the second manifold (921); the liquid outlet of the second delivery pump (922) is connected to the feed end of the second temperature control pipe (923); the second Temperature control fitting (923) is used to adjust and control the temperature of the liquid material formed by mixing the ethylene oxide conveyed by the ethylene oxide storage tank (5), the propylene oxide conveyed by the propylene oxide storage tank (6), and the intermediate reaction production material conveyed by the discharge pipe (404) of the upstream monomer reactor unit assembly (40) through the second manifold (921) and the second delivery pump (922). By controlling the mass ratio of the ethylene oxide conveyed by the ethylene oxide storage tank (5) and the propylene oxide conveyed by the propylene oxide storage tank (6), ethoxylated polyether products with different block structures can be formed.

7. A continuous ethoxylation reaction apparatus according to claim 4, characterized in that: The inner and outer walls of the guide tube (403) are integrally formed with a number of first heat dissipation strips (4031) that are consistent with the axial direction of the guide tube (403).

8. A continuous ethoxylation reaction apparatus according to claim 4, characterized in that: The inner and outer walls of the reaction tube (401) are integrally formed with several second heat dissipation strips (4011) that are aligned with the axial direction of the reaction tube (401).

Images