Three-phase multi-section fluidized bed reactor and rectification coupling continuous esterification reaction rectification device
Through a continuous esterification reaction distillation device coupled with a three-phase multi-stage fluidized bed reactor and distillation, the problem of complex process and low raw material utilization of the fluidized bed reactor and distillation tower coupling device is solved, and efficient esterification reaction and raw material reflux are achieved, which improves the reaction conversion rate and reduces energy consumption.
Patent Information
- Application Number
- CN202510939802.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-09
- Publication Date
- 2025-08-19
AI Technical Summary
In the prior art, the coupling device between the fluidized bed reactor and the distillation tower has problems such as complex flow, low operating elasticity, low raw material utilization rate and low reaction conversion rate.
A continuous esterification reaction distillation device coupled with distillation is designed. The three-phase multi-stage fluidized bed reactor is formed in the multi-stage fluidized bed reactor to carry out the esterification reaction by forming a gas-liquid-solid three-phase fluidized bed reactor, and the aqueous phase and oil phase are automatically produced by an automatic phase separator. The unreacted raw materials are condensed through the distillation tower and gravity reflux into the reaction section to continue the reaction, and the multi-stage fluidized bed reactor is combined as the tower kettle of the distillation tower to provide a heating heat source.
It achieves simple process, high operational flexibility, high raw material utilization rate and high reaction conversion rate, reducing energy consumption and saving equipment space and construction investment.
Smart Images
Figure CN120502287A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a three-phase multi-stage fluidized bed reactor and a rectification coupled continuous esterification reaction rectification device, belonging to the technical field of chemical reaction and separation coupling. Background Art
[0002] A fluidized bed reactor is a highly efficient multiphase reaction device that achieves efficient mass transfer, heat transfer, and chemical reactions by suspending solid particles (such as catalysts or reactants) in a flowing gas or liquid to form a gas-solid, liquid-solid, or gas-solid-liquid "fluidization."
[0003] Distillation tower is one of the most core equipment in the chemical separation process. It is used to achieve efficient separation of mixtures through mass and heat transfer between vapor and liquid phases. It is widely used in petroleum refining, chemical production, pharmaceuticals, food processing and environmental protection.
[0004] The organic combination of a fluidized bed reactor and a distillation tower is an enhanced technology that couples chemical reactions with process separation. The distillation tower can achieve in-situ selective separation of products. At the same time, optimizing the reflux strategy can significantly improve the reaction conversion rate, product selectivity and energy utilization, realizing the triple synergy of reaction, separation and energy utilization, and achieving the goal of energy conservation and emission reduction. Summary of the Invention
[0005] The technical problem to be solved by the present invention is to provide a continuous esterification reaction distillation device coupled with a three-phase multi-stage fluidized bed reactor and distillation, which has simple process, large operation flexibility, energy saving and consumption reduction, high raw material utilization rate and high reaction conversion rate.
[0006] The three-phase multi-stage fluidized bed reactor and distillation coupled continuous esterification reaction distillation device of the present invention comprises a multi-stage fluidized bed reactor (1), a distillation tower (2), a reaction section 1 (3), a reaction section 2 (4), a reaction section 3 (5), a reaction section 1 heater (6), a reaction section 2 heater (7), a reaction section 3 heater (8), a tower top condenser (9), an automatic phase separator (10), an aqueous phase collecting tank (11), a reflux ratio controller (12), a material reflux valve (13), a nitrogen inlet valve (14), a raw material feed pump (15), a raw material The feed valve (16) and the product extraction valve (17) are characterized in that: the esterification reaction distillation device of the three-phase multi-stage fluidized bed reactor coupled with the distillation is composed of a multi-stage fluidized bed reactor (1) and a distillation tower (2), the top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation tower (2), the multi-stage fluidized bed reactor (1) is divided into reaction section 1 (3), reaction section 2 (4) and reaction section 3 (5) from bottom to top, the reaction section 1 (3) is provided with a reaction section 1 heater (6) outside, the reaction section 2 (4) is provided with a reaction section 1 heater (6) outside. The reaction section 2 heater (7) is provided outside the reaction section 3 (5). The top of the distillation tower (2) is connected to the tower top condenser (9) and the automatic phase separator (10) in sequence through pipelines. The material is condensed by the tower top condenser (9) and is divided into two streams. One stream flows back to the distillation tower (2) through the reflux ratio controller (12) to maintain the normal operation of the distillation tower (2), and the other stream flows to the automatic phase separator (10) to form a water phase and an oil phase in the automatic phase separator (10). The characteristics of the internal components of the automatic phase separator (10) are utilized. The special structure is that the water phase is automatically and continuously extracted and flows into the water phase collection tank (11); the oil phase is automatically and continuously extracted and flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material reflux valve (13) to continue to participate in the reaction; N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14); the reaction raw materials are fed through the raw material feed pump (15); the outlet of the raw material feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through a pipeline; the high boiling point product is extracted from the reaction section 3 (5) through the product extraction valve (17).
[0007] The multi-stage fluidized bed reactor (1) is fluidized in a gas-liquid-solid three-phase state by solid, liquid and N2 to carry out the esterification reaction. The solid includes: a catalyst or a raw solid acid; the liquid includes: a raw liquid acid or a liquid fatty alcohol with a carbon number greater than 4; the boiling points of the raw alcohol and the raw acid are higher than water; the catalyst is a solid particle catalyst or a catalyst miscible with the liquid raw material; N2 is used as a fluidizing gas and can also be replaced by other gases participating in the reaction.
[0008] Reaction sections 1 (3), 2 (4) and 3 (5) of different diameters are designed according to the density of the solid material and the catalyst particles. Materials of different particles have different fluidization velocities in each section and participate in the reaction in different reaction sections.
[0009] The three-phase multi-stage fluidized bed reactor and distillation coupling continuous esterification reaction distillation device has an operating temperature of 50°C to 300°C and an operating pressure of vacuum, normal pressure or pressurized pressure.
[0010] The beneficial effects of the present invention are: 1. This device can automatically extract the water produced by the esterification reaction through the special structure of the internal components of the automatic phase separator (10), pushing the reaction in the positive direction, thereby breaking the equilibrium conversion rate.
[0011] 2. This device can condense the unreacted raw materials during the esterification reaction at the top of the distillation tower (2), automatically separate the phases, and then automatically flow back to the reaction section (1) by gravity to continue the reaction, thereby improving the raw material utilization rate and the reaction conversion rate, and making the reaction conversion rate exceed the equilibrium conversion rate.
[0012] 3. The diameters of reaction section 1 (3), reaction section 2 (4) and reaction section 3 (5) are different. According to the density of the solid material and the design of the catalyst particles, the materials with different particles have different fluidization velocities in each section. At the same time, each reaction section is also equipped with an independent heater outside. The temperature of the heater is set according to the different reactions in each section, and the device has great operational flexibility.
[0013] 4. This device integrates a multi-stage fluidized bed reactor (1) and a distillation tower (2). The multi-stage fluidized bed reactor (1) serves as the bottom of the distillation tower (2) to provide a heating source for the distillation tower (2). The unreacted raw materials separated by the distillation tower (2) flow back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) by gravity to participate in the reaction again, thereby achieving a synergistic effect of reaction promoting separation and separation promoting reaction, further improving the reaction rate. At the same time, the reaction energy consumption is reduced, and equipment space and construction investment are saved. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 It is a schematic diagram of the structure of a continuous esterification reaction distillation device with a three-phase multi-stage fluidized bed reactor coupled with distillation. DETAILED DESCRIPTION
[0015] To make the present invention more clearly understood, preferred embodiments are described in detail below with reference to the accompanying drawings, but the present invention is not limited thereto.
[0016] Example 1: In this embodiment, Figure 1The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction distillation device is composed of a multi-stage fluidized bed reactor (1), a distillation tower (2), a reaction section 1 (3), a reaction section 2 (4), a reaction section 3 (5), a reaction section 1 heater (6), a reaction section 2 heater (7), a reaction section 3 heater (8), a tower top condenser (9), an automatic phase separator (10), an aqueous phase collection tank (11), a reflux ratio controller (12), a material reflux valve (13), a nitrogen inlet valve (14), a raw material feed pump (15), a raw material feed valve (16) and a product extraction valve (17). The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction distillation device is composed of a multi-stage fluidized bed reactor (1) and a distillation tower (2 ), the top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation tower (2), and the multi-stage fluidized bed reactor (1) is composed of reaction section 1 (3), reaction section 2 (4) and reaction section 3 (5) from bottom to top. Reaction sections 1 (3), reaction section 2 (4) and reaction section 3 (5) with different diameters are designed according to the density of the solid material and the catalyst particles. Materials with different particles have different fluidization speeds in each section and participate in the reaction in different reaction sections. A reaction section 1 heater (6) is provided outside the reaction section 1 (3), a reaction section 2 heater (7) is provided outside the reaction section 2 (4), and a reaction section 3 heater (8) is provided outside the reaction section 3 (5). The top of the distillation tower (2) is connected to the top condenser ( 9) and an automatic phase separator (10). The material is condensed by the tower top condenser (9) and is divided into two streams. One stream flows back to the distillation tower (2) through the reflux ratio controller (12) to maintain the normal operation of the distillation tower (2), and the other stream flows to the automatic phase separator (10). A water phase and an oil phase are formed in the automatic phase separator (10). By utilizing the special structure of the internal components of the automatic phase separator (10), the water phase is automatically and continuously extracted and flows into the water phase collection tank (11). After the oil phase is automatically and continuously extracted, it flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material reflux valve (13) to continue to participate in the reaction. N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14). The reaction raw materials are fed through the raw material feed pump (15). The outlet of the feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through a pipeline. The high boiling point product is extracted from the reaction section 3 (5) through the product extraction valve (17). The solid, liquid and N2 form a gas-liquid-solid three-phase fluidization in the multi-stage fluidized bed reactor (1) to carry out the esterification reaction. The solid includes: a catalyst or a raw material solid acid, and the liquid includes: a raw material liquid acid or a liquid fatty alcohol with a carbon number greater than 4. The boiling point of the raw material alcohol and the raw material acid is higher than that of water. The catalyst is a solid particle catalyst or a catalyst miscible with the liquid raw material. N2 is used as a fluidizing gas and can also be replaced by other gases participating in the reaction. The operating temperature of the device is: 50℃~300℃, and the operating pressure is: vacuum or normal pressure or pressurized.
Claims
1. A three-phase multi-stage fluidized bed reactor coupled with distillation for continuous esterification reaction and distillation, comprising a multi-stage fluidized bed reactor (1), a distillation tower (2), a reaction section 1 (3), a reaction section 2 (4), a reaction section 3 (5), a heater for reaction section 1 (6), a heater for reaction section 2 (7), a heater for reaction section 3 (8), a tower top condenser (9), an automatic phase separator (10), an aqueous phase collecting tank (11), a reflux ratio controller (12), a material reflux valve (13), a nitrogen inlet valve (14), a raw material feed pump (15), a raw material feed valve (16) and a product extraction valve (17), characterized in that: The esterification reaction distillation device coupled with a three-phase multi-stage fluidized bed reactor and distillation comprises a multi-stage fluidized bed reactor (1) and a distillation tower (2). The top of the multi-stage fluidized bed reactor (1) is connected to the bottom of the distillation tower (2). The multi-stage fluidized bed reactor (1) is composed of a reaction section 1 (3), a reaction section 2 (4) and a reaction section 3 (5) from bottom to top. The reaction section 1 (3) is provided with a reaction section 1 heater (6) outside, the reaction section 2 (4) is provided with a reaction section 2 heater (7) outside, and the reaction section 3 (5) is provided with a reaction section 3 heater (8) outside. The top of the distillation tower (2) is connected to a tower top condenser (9) and an automatic phase separator (10) in sequence through pipelines. After condensation by the tower top condenser (9), the material is divided into two streams, one of which is condensed by a reflux ratio control device. The liquid flows back to the distillation tower (2) through the control device (12), and the normal operation of the distillation tower (2) is maintained. One stream flows to the automatic phase separator (10), and a water phase and an oil phase are formed in the automatic phase separator (10). By utilizing the special structure of the internal components of the automatic phase separator (10), the water phase is automatically and continuously extracted and flows into the water phase collection tank (11). After the oil phase is automatically and continuously extracted, it flows back to the reaction section 1 (3) of the multi-stage fluidized bed reactor (1) through the material reflux valve (13) to continue to participate in the reaction. N2 enters from the bottom of the reaction section 1 (3) through the nitrogen inlet valve (14). The reaction raw materials are fed through the raw material feed pump (15). The outlet of the raw material feed pump (15) is connected to the raw material feed valve (16) and the reaction section 1 (3) in sequence through a pipeline. The high-boiling-point product is extracted from the reaction section 3 (5) through the product extraction valve (17).
2. The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction and distillation device according to claim 1, characterized in that: The multi-stage fluidized bed reactor (1) is fluidized in a gas-liquid-solid three-phase state by solid, liquid and N2 to carry out the esterification reaction. The solid includes: a catalyst or a raw solid acid; the liquid includes: a raw liquid acid or a liquid fatty alcohol with a carbon number greater than 4; the boiling points of the raw alcohol and the raw acid are higher than water; the catalyst is a solid particle catalyst or a catalyst miscible with the liquid raw material; N2 is used as a fluidizing gas and can also be replaced by other gases participating in the reaction.
3. The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction and distillation device according to claim 1, characterized in that: Reaction sections 1 (3), 2 (4) and 3 (5) of different diameters are designed according to the density of the solid material and the catalyst particles. Materials of different particles have different fluidization velocities in each section and participate in the reaction in different reaction sections.
4. The three-phase multi-stage fluidized bed reactor coupled with distillation continuous esterification reaction and distillation device according to claim 1, characterized in that: The device can be used at a temperature of 50°C to 300°C and at a pressure of vacuum, normal pressure or pressurized pressure.